The combination of cobalt, 3,5-di-tert-butyldioxolene (3,5-dbdiox) and 1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane (tpch) yields two coordination polymers with different connectivities, i.e. a one-dimensional zigzag chain and a two-dimensional sheet. Poly[[bis(3,5-di-tert-butylbenzene-1,2-diolato)bis(1,5-di-tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)[μ4-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]cobalt(III)]–ethanol–water 1/7/5], {[Co2(C14H20O2)4(C26H24N4O)]·7C2H5OH·5H2O}n or {[Co2(3,5-dbdiox)4(tpch)}·7EtOH·5H2O}n, is the second structurally characterized example of a two-dimensional coordination polymer based on linked {Co(3,5-dbdiox)2} units. Variable-temperature single-crystal X-ray diffraction studies suggest that catena-poly[[[(3,5-di-tert-butylbenzene-1,2-diolato)(1,5-di-tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)cobalt(III)]-μ-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]–ethanol–water (1/1/5)], {[Co(C14H20O2)2(C26H24N4O)]·C2H5OH·5H2O}n or {[Co(3,5-dbdiox)2(tpch)]·EtOH·5H2O}n, undergoes a temperature-induced valence tautomeric interconversion.
Supporting information
CCDC references: 1840985; 1840984; 1840983; 1840982
For all structures, data collection: BluIce (McPhillips et al., 2002); cell refinement: XDS (Kabsch, 1993); data reduction: XDS (Kabsch, 1993); program(s) used to solve structure: SHELXT (Sheldrick, 2015a). Program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b) for 1_100K; SHELXL (Sheldrick, 2015b) for 2_100k, 2_275k; SHELXL2018 (Sheldrick, 2015b) for 2_315k. For all structures, molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
Poly[[bis(3,5-di-
tert-butylbenzene-1,2-diolato)bis(1,5-di-
tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)[µ
4-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]cobalt(III)]–ethanol–water 1/7/5] (1_100K)
top
Crystal data top
[Co2(C14H20O2)4(C26H24N4O)]·7C2H6O·5H2O | F(000) = 1964 |
Mr = 1820.10 | Dx = 1.190 Mg m−3 |
Monoclinic, P21/c | Synchrotron radiation, λ = 0.71073 Å |
a = 23.849 (5) Å | Cell parameters from 60678 reflections |
b = 11.679 (2) Å | θ = 2.1–26.5° |
c = 18.319 (4) Å | µ = 0.39 mm−1 |
β = 95.28 (3)° | T = 100 K |
V = 5080.8 (18) Å3 | Plate, clear blue |
Z = 2 | 0.1 × 0.07 × 0.02 mm |
Data collection top
ADSC Quantum 210r diffractometer | 10426 independent reflections |
Radiation source: MX1 Beamline Australian Synchrotron | 7436 reflections with I > 2σ(I) |
Silicon Double Crystal monochromator | Rint = 0.093 |
Phi Scan scans | θmax = 26.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2012) | h = −29→29 |
Tmin = 0.583, Tmax = 0.745 | k = −14→14 |
73724 measured reflections | l = −22→22 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.081 | w = 1/[σ2(Fo2) + (0.106P)2 + 8.894P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.231 | (Δ/σ)max = 0.001 |
S = 1.05 | Δρmax = 1.09 e Å−3 |
10426 reflections | Δρmin = −0.73 e Å−3 |
526 parameters | Extinction correction: SHELXL2014 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
21 restraints | Extinction coefficient: 0.0163 (13) |
Primary atom site location: dual | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Crystals were small and weakly scattering, hence data collection was carried
out at the Australian Synchrotron. Some of the crystals were disordered, the
crystals showed minor disorder, however the Rint value was still relatively
high. During the refinement it was found the structure was disordered: the
alcohol group of the tpch ligand is disordered over four positions on the
cyclohexane ring and so refinement was carried out with these atoms restrained
to ideal geometry. One of the tert-butyl groups also displays disorder and so
refinement was carried out with these groups disordered over two components,
both being restrained to ideal geometry. The maximum residual electron
density peaks, of around 1.1 eA-3, were close to atoms of the cyclohexane ring
of the tpch ligand indicating that this group was somewhat disordered.
Attempts to model this disorder were not successful. The disorder required a
number of distance and angle constraints and restraints to ensure the
disordered components were maintained at a chemical reasonable geometry. The
displacement parameters of each of the atoms of each component were
constrained to be equal. The crystal showed a solvent void containing
disordered/diffuse solvent consistent with 15 molecules of water per formula
unit (containing two cobalt atoms), or a mixture of 5 molecules of ethanol and
5 molecules of water. There were three reflections OMITted due to anomalous
background. The high final R and wR values are a consequence of the disorder
of the crystals. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.27666 (2) | 0.29489 (5) | 0.20493 (3) | 0.03957 (19) | |
O3 | 0.22768 (11) | 0.3754 (2) | 0.25882 (14) | 0.0404 (6) | |
O2 | 0.21382 (11) | 0.2570 (2) | 0.13879 (14) | 0.0398 (6) | |
O1 | 0.25713 (11) | 0.1621 (2) | 0.25759 (14) | 0.0416 (6) | |
O4 | 0.28641 (11) | 0.4303 (3) | 0.15159 (16) | 0.0480 (7) | |
N1 | 0.33676 (14) | 0.3343 (4) | 0.28049 (19) | 0.0497 (9) | |
N2 | 0.32906 (14) | 0.2877 (3) | 0.64715 (18) | 0.0483 (9) | |
C4 | 0.08897 (16) | 0.1284 (3) | 0.2012 (2) | 0.0394 (8) | |
H4 | 0.0496 | 0.1203 | 0.1886 | 0.047* | |
C1 | 0.20266 (15) | 0.1479 (3) | 0.2430 (2) | 0.0378 (8) | |
C15 | 0.21382 (16) | 0.4741 (3) | 0.22473 (19) | 0.0377 (8) | |
C3 | 0.11944 (16) | 0.1865 (3) | 0.1534 (2) | 0.0385 (8) | |
C2 | 0.17848 (16) | 0.1995 (3) | 0.1760 (2) | 0.0374 (8) | |
C6 | 0.16887 (16) | 0.0874 (3) | 0.2878 (2) | 0.0397 (8) | |
H6 | 0.1852 | 0.0520 | 0.3314 | 0.048* | |
O7 | 0.31575 (19) | 0.0520 (5) | 0.5125 (2) | 0.0918 (13) | |
H7 | 0.3087 | 0.0728 | 0.5545 | 0.138* | |
C5 | 0.11204 (16) | 0.0791 (3) | 0.2690 (2) | 0.0385 (8) | |
C16 | 0.24383 (17) | 0.5023 (4) | 0.1645 (2) | 0.0445 (9) | |
C17 | 0.23090 (19) | 0.6003 (4) | 0.1237 (2) | 0.0491 (10) | |
H17 | 0.2512 | 0.6178 | 0.0829 | 0.059* | |
C25 | 0.14328 (17) | 0.5238 (4) | 0.3171 (2) | 0.0424 (9) | |
C20 | 0.17258 (16) | 0.5498 (3) | 0.2477 (2) | 0.0403 (9) | |
C19 | 0.16035 (19) | 0.6477 (4) | 0.2044 (2) | 0.0464 (9) | |
H19 | 0.1320 | 0.6984 | 0.2180 | 0.056* | |
C27 | 0.11259 (17) | 0.4072 (4) | 0.3091 (2) | 0.0443 (9) | |
H27A | 0.0874 | 0.4068 | 0.2637 | 0.066* | |
H27B | 0.0905 | 0.3954 | 0.3510 | 0.066* | |
H27C | 0.1404 | 0.3457 | 0.3075 | 0.066* | |
C8 | 0.03018 (16) | 0.2110 (4) | 0.0677 (2) | 0.0456 (9) | |
H8A | 0.0247 | 0.1279 | 0.0668 | 0.068* | |
H8B | 0.0156 | 0.2435 | 0.0204 | 0.068* | |
H8C | 0.0100 | 0.2445 | 0.1068 | 0.068* | |
C28 | 0.18800 (19) | 0.5180 (4) | 0.3820 (2) | 0.0482 (10) | |
H28A | 0.2159 | 0.4594 | 0.3727 | 0.072* | |
H28B | 0.1702 | 0.4984 | 0.4265 | 0.072* | |
H28C | 0.2067 | 0.5926 | 0.3885 | 0.072* | |
C9 | 0.10053 (18) | 0.3698 (4) | 0.0835 (2) | 0.0467 (10) | |
H9A | 0.0827 | 0.4011 | 0.1253 | 0.070* | |
H9B | 0.0825 | 0.4023 | 0.0379 | 0.070* | |
H9C | 0.1406 | 0.3895 | 0.0883 | 0.070* | |
C7 | 0.09386 (16) | 0.2383 (4) | 0.0820 (2) | 0.0401 (9) | |
C26 | 0.1007 (2) | 0.6148 (4) | 0.3327 (2) | 0.0514 (10) | |
H26A | 0.1201 | 0.6879 | 0.3426 | 0.077* | |
H26B | 0.0816 | 0.5923 | 0.3756 | 0.077* | |
H26C | 0.0730 | 0.6230 | 0.2901 | 0.077* | |
C41 | 0.37664 (18) | 0.2377 (5) | 0.6302 (2) | 0.0578 (12) | |
H41 | 0.3852 | 0.1624 | 0.6474 | 0.069* | |
C18 | 0.1879 (2) | 0.6740 (4) | 0.1425 (2) | 0.0502 (10) | |
C10 | 0.12290 (19) | 0.1868 (4) | 0.0182 (2) | 0.0539 (11) | |
H10A | 0.1635 | 0.2008 | 0.0260 | 0.081* | |
H10B | 0.1078 | 0.2225 | −0.0279 | 0.081* | |
H10C | 0.1159 | 0.1041 | 0.0158 | 0.081* | |
C13 | 0.02965 (19) | 0.1097 (4) | 0.3412 (3) | 0.0539 (11) | |
H13A | 0.0499 | 0.1678 | 0.3718 | 0.081* | |
H13B | 0.0019 | 0.0719 | 0.3692 | 0.081* | |
H13C | 0.0104 | 0.1463 | 0.2977 | 0.081* | |
C12 | 0.0400 (2) | −0.0763 (4) | 0.2745 (3) | 0.0567 (11) | |
H12A | 0.0227 | −0.0465 | 0.2277 | 0.085* | |
H12B | 0.0106 | −0.1063 | 0.3033 | 0.085* | |
H12C | 0.0664 | −0.1379 | 0.2653 | 0.085* | |
C11 | 0.07173 (18) | 0.0201 (4) | 0.3172 (2) | 0.0474 (10) | |
C14 | 0.1028 (2) | −0.0317 (4) | 0.3864 (2) | 0.0552 (11) | |
H14A | 0.1296 | −0.0895 | 0.3725 | 0.083* | |
H14B | 0.0755 | −0.0676 | 0.4162 | 0.083* | |
H14C | 0.1231 | 0.0288 | 0.4149 | 0.083* | |
C29 | 0.36955 (18) | 0.2557 (5) | 0.3154 (2) | 0.0555 (11) | |
H29 | 0.3656 | 0.1784 | 0.2997 | 0.067* | |
C35 | 0.5061 (2) | 0.4970 (6) | 0.4226 (2) | 0.0693 (16) | |
H35A | 0.4877 | 0.5698 | 0.4063 | 0.083* | |
H35B | 0.5196 | 0.4588 | 0.3793 | 0.083* | |
C40 | 0.3175 (2) | 0.3932 (4) | 0.6200 (2) | 0.0573 (12) | |
H40 | 0.2834 | 0.4288 | 0.6307 | 0.069* | |
C30 | 0.3427 (2) | 0.4425 (5) | 0.3025 (3) | 0.0604 (12) | |
H30 | 0.3197 | 0.4996 | 0.2779 | 0.072* | |
C39 | 0.41384 (19) | 0.2930 (6) | 0.5882 (3) | 0.0757 (18) | |
H39 | 0.4475 | 0.2557 | 0.5773 | 0.091* | |
C42 | 0.2693 (2) | 0.2216 (6) | 0.4569 (3) | 0.0771 (17) | |
H42A | 0.2418 | 0.2451 | 0.4166 | 0.116* | |
H42B | 0.3063 | 0.2535 | 0.4492 | 0.116* | |
H42C | 0.2574 | 0.2501 | 0.5034 | 0.116* | |
C21 | 0.1714 (2) | 0.7768 (4) | 0.0946 (2) | 0.0568 (12) | |
C32 | 0.3817 (2) | 0.4749 (6) | 0.3605 (3) | 0.0731 (16) | |
H32 | 0.3850 | 0.5528 | 0.3752 | 0.088* | |
C38 | 0.3528 (2) | 0.4525 (6) | 0.5774 (3) | 0.0717 (16) | |
H38 | 0.3427 | 0.5266 | 0.5592 | 0.086* | |
C31 | 0.4088 (2) | 0.2806 (6) | 0.3730 (3) | 0.0704 (16) | |
H31 | 0.4309 | 0.2211 | 0.3964 | 0.084* | |
C33 | 0.4159 (2) | 0.3907 (6) | 0.3965 (3) | 0.0729 (17) | |
C37 | 0.4019 (2) | 0.4041 (6) | 0.5618 (3) | 0.0757 (18) | |
C34 | 0.4628 (2) | 0.4182 (6) | 0.4574 (3) | 0.089 (2) | |
H34 | 0.4818 | 0.3456 | 0.4748 | 0.107* | 0.75 |
C36 | 0.4426 (2) | 0.4777 (5) | 0.5192 (3) | 0.0792 (18) | |
H36 | 0.4239 | 0.5510 | 0.5025 | 0.095* | 0.75 |
C43 | 0.2729 (3) | 0.0945 (7) | 0.4592 (3) | 0.100 (2) | |
H43A | 0.2360 | 0.0634 | 0.4704 | 0.119* | |
H43B | 0.2804 | 0.0661 | 0.4102 | 0.119* | |
C24 | 0.1488 (3) | 0.7369 (6) | 0.0175 (3) | 0.059 (2) | 0.708 (8) |
H24A | 0.1773 | 0.6901 | −0.0036 | 0.088* | 0.708 (8) |
H24B | 0.1400 | 0.8039 | −0.0138 | 0.088* | 0.708 (8) |
H24C | 0.1145 | 0.6914 | 0.0207 | 0.088* | 0.708 (8) |
C23 | 0.2242 (5) | 0.8561 (7) | 0.0874 (5) | 0.094 (4) | 0.708 (8) |
H23A | 0.2386 | 0.8836 | 0.1360 | 0.141* | 0.708 (8) |
H23B | 0.2131 | 0.9215 | 0.0558 | 0.141* | 0.708 (8) |
H23C | 0.2536 | 0.8123 | 0.0658 | 0.141* | 0.708 (8) |
C22 | 0.1254 (5) | 0.8545 (7) | 0.1230 (5) | 0.092 (4) | 0.708 (8) |
H22A | 0.0895 | 0.8131 | 0.1201 | 0.138* | 0.708 (8) |
H22B | 0.1212 | 0.9238 | 0.0929 | 0.138* | 0.708 (8) |
H22C | 0.1364 | 0.8758 | 0.1741 | 0.138* | 0.708 (8) |
O6 | 0.4911 (5) | 0.3165 (9) | 0.4878 (8) | 0.066 (4) | 0.25 |
H6A | 0.5256 | 0.3301 | 0.4969 | 0.100* | 0.25 |
O5 | 0.4158 (4) | 0.5811 (8) | 0.4890 (6) | 0.046 (3) | 0.25 |
H5 | 0.4316 | 0.6386 | 0.5093 | 0.069* | 0.25 |
C22A | 0.1880 (8) | 0.8759 (15) | 0.1442 (10) | 0.063 (5) | 0.292 (8) |
H22D | 0.1742 | 0.8629 | 0.1923 | 0.095* | 0.292 (8) |
H22E | 0.1715 | 0.9466 | 0.1229 | 0.095* | 0.292 (8) |
H22F | 0.2291 | 0.8830 | 0.1498 | 0.095* | 0.292 (8) |
C23A | 0.1090 (11) | 0.7717 (18) | 0.0724 (11) | 0.093 (8) | 0.292 (8) |
H23D | 0.1009 | 0.7081 | 0.0382 | 0.139* | 0.292 (8) |
H23E | 0.0967 | 0.8438 | 0.0487 | 0.139* | 0.292 (8) |
H23F | 0.0888 | 0.7599 | 0.1161 | 0.139* | 0.292 (8) |
C24A | 0.2028 (11) | 0.7760 (19) | 0.0248 (12) | 0.085 (7) | 0.292 (8) |
H24D | 0.2425 | 0.7952 | 0.0376 | 0.127* | 0.292 (8) |
H24E | 0.1858 | 0.8325 | −0.0100 | 0.127* | 0.292 (8) |
H24F | 0.2001 | 0.6997 | 0.0025 | 0.127* | 0.292 (8) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0303 (3) | 0.0530 (3) | 0.0359 (3) | 0.0003 (2) | 0.00554 (19) | −0.0032 (2) |
O3 | 0.0390 (14) | 0.0482 (16) | 0.0345 (14) | −0.0006 (12) | 0.0067 (11) | 0.0028 (12) |
O2 | 0.0348 (13) | 0.0526 (16) | 0.0329 (14) | 0.0050 (12) | 0.0076 (10) | 0.0024 (12) |
O1 | 0.0313 (13) | 0.0531 (16) | 0.0401 (15) | 0.0060 (12) | 0.0013 (11) | −0.0023 (12) |
O4 | 0.0384 (15) | 0.0581 (18) | 0.0498 (17) | −0.0013 (13) | 0.0151 (12) | 0.0027 (14) |
N1 | 0.0365 (18) | 0.072 (2) | 0.0419 (19) | −0.0074 (17) | 0.0118 (14) | −0.0056 (18) |
N2 | 0.0320 (17) | 0.074 (3) | 0.0392 (18) | −0.0070 (16) | 0.0042 (13) | 0.0039 (17) |
C4 | 0.0315 (18) | 0.046 (2) | 0.041 (2) | 0.0000 (16) | 0.0032 (15) | −0.0018 (17) |
C1 | 0.0333 (19) | 0.042 (2) | 0.038 (2) | 0.0022 (15) | 0.0034 (15) | −0.0031 (16) |
C15 | 0.043 (2) | 0.044 (2) | 0.0279 (18) | −0.0045 (16) | 0.0081 (15) | −0.0009 (15) |
C3 | 0.0383 (19) | 0.040 (2) | 0.037 (2) | 0.0012 (16) | 0.0020 (15) | −0.0056 (16) |
C2 | 0.0365 (19) | 0.044 (2) | 0.0326 (19) | 0.0022 (16) | 0.0068 (14) | −0.0039 (16) |
C6 | 0.041 (2) | 0.037 (2) | 0.040 (2) | 0.0004 (16) | 0.0029 (16) | 0.0015 (16) |
O7 | 0.092 (3) | 0.128 (4) | 0.057 (2) | 0.010 (3) | 0.015 (2) | 0.003 (2) |
C5 | 0.0395 (19) | 0.0360 (19) | 0.040 (2) | 0.0001 (15) | 0.0044 (15) | −0.0037 (16) |
C16 | 0.041 (2) | 0.051 (2) | 0.042 (2) | −0.0080 (18) | 0.0065 (17) | −0.0048 (18) |
C17 | 0.059 (3) | 0.053 (2) | 0.036 (2) | −0.013 (2) | 0.0097 (18) | 0.0006 (18) |
C25 | 0.043 (2) | 0.048 (2) | 0.037 (2) | −0.0019 (17) | 0.0101 (16) | −0.0046 (17) |
C20 | 0.042 (2) | 0.044 (2) | 0.035 (2) | −0.0012 (17) | 0.0048 (15) | −0.0040 (16) |
C19 | 0.056 (2) | 0.046 (2) | 0.037 (2) | 0.0010 (19) | 0.0025 (18) | −0.0025 (18) |
C27 | 0.041 (2) | 0.050 (2) | 0.043 (2) | −0.0007 (18) | 0.0110 (16) | −0.0020 (18) |
C8 | 0.039 (2) | 0.057 (3) | 0.040 (2) | −0.0006 (18) | −0.0005 (16) | 0.0042 (19) |
C28 | 0.058 (3) | 0.056 (3) | 0.031 (2) | −0.005 (2) | 0.0068 (17) | 0.0009 (18) |
C9 | 0.046 (2) | 0.052 (2) | 0.042 (2) | 0.0020 (19) | 0.0026 (17) | 0.0043 (18) |
C7 | 0.0366 (19) | 0.049 (2) | 0.035 (2) | 0.0056 (16) | 0.0030 (15) | 0.0003 (16) |
C26 | 0.063 (3) | 0.046 (2) | 0.047 (2) | 0.008 (2) | 0.015 (2) | −0.0036 (19) |
C41 | 0.037 (2) | 0.094 (4) | 0.044 (2) | −0.005 (2) | 0.0086 (18) | 0.006 (2) |
C18 | 0.065 (3) | 0.046 (2) | 0.039 (2) | −0.008 (2) | 0.0021 (19) | −0.0050 (18) |
C10 | 0.047 (2) | 0.076 (3) | 0.040 (2) | 0.010 (2) | 0.0059 (18) | −0.009 (2) |
C13 | 0.048 (2) | 0.063 (3) | 0.053 (3) | 0.002 (2) | 0.0145 (19) | 0.001 (2) |
C12 | 0.053 (3) | 0.057 (3) | 0.060 (3) | −0.010 (2) | 0.003 (2) | 0.005 (2) |
C11 | 0.043 (2) | 0.056 (3) | 0.044 (2) | −0.0031 (19) | 0.0054 (17) | 0.0036 (19) |
C14 | 0.059 (3) | 0.059 (3) | 0.048 (3) | −0.003 (2) | 0.008 (2) | 0.009 (2) |
C29 | 0.037 (2) | 0.083 (3) | 0.046 (2) | −0.007 (2) | 0.0001 (18) | 0.003 (2) |
C35 | 0.047 (3) | 0.122 (5) | 0.040 (2) | −0.037 (3) | 0.0050 (19) | −0.003 (3) |
C40 | 0.057 (3) | 0.069 (3) | 0.046 (2) | −0.018 (2) | 0.007 (2) | 0.009 (2) |
C30 | 0.049 (3) | 0.069 (3) | 0.063 (3) | −0.015 (2) | 0.005 (2) | −0.012 (2) |
C39 | 0.029 (2) | 0.145 (6) | 0.053 (3) | −0.015 (3) | 0.0086 (19) | −0.016 (3) |
C42 | 0.055 (3) | 0.126 (6) | 0.052 (3) | 0.001 (3) | 0.012 (2) | −0.007 (3) |
C21 | 0.083 (3) | 0.046 (3) | 0.042 (2) | 0.002 (2) | 0.008 (2) | 0.0017 (19) |
C32 | 0.062 (3) | 0.099 (4) | 0.060 (3) | −0.038 (3) | 0.016 (3) | −0.024 (3) |
C38 | 0.064 (3) | 0.095 (4) | 0.055 (3) | −0.032 (3) | 0.001 (2) | 0.014 (3) |
C31 | 0.046 (3) | 0.120 (5) | 0.043 (3) | −0.024 (3) | −0.004 (2) | 0.015 (3) |
C33 | 0.046 (3) | 0.134 (5) | 0.039 (2) | −0.036 (3) | 0.007 (2) | 0.012 (3) |
C37 | 0.065 (3) | 0.121 (5) | 0.039 (3) | −0.049 (3) | −0.001 (2) | 0.003 (3) |
C34 | 0.070 (3) | 0.154 (6) | 0.042 (3) | −0.065 (4) | 0.003 (2) | −0.002 (3) |
C36 | 0.060 (3) | 0.124 (5) | 0.054 (3) | −0.043 (3) | 0.006 (2) | −0.002 (3) |
C43 | 0.119 (6) | 0.115 (6) | 0.058 (4) | −0.021 (5) | −0.029 (4) | 0.010 (4) |
C24 | 0.081 (5) | 0.054 (4) | 0.039 (3) | −0.002 (3) | −0.003 (3) | 0.003 (3) |
C23 | 0.127 (8) | 0.064 (5) | 0.084 (6) | −0.043 (5) | −0.024 (6) | 0.027 (5) |
C22 | 0.165 (11) | 0.057 (5) | 0.058 (5) | 0.034 (6) | 0.026 (5) | 0.012 (4) |
O6 | 0.059 (6) | 0.083 (7) | 0.054 (6) | −0.016 (6) | −0.011 (5) | 0.026 (6) |
O5 | 0.040 (5) | 0.063 (6) | 0.034 (5) | −0.009 (5) | −0.001 (4) | 0.019 (5) |
C22A | 0.061 (11) | 0.058 (10) | 0.071 (12) | 0.005 (8) | 0.008 (9) | −0.011 (8) |
C23A | 0.15 (2) | 0.066 (13) | 0.056 (12) | 0.046 (13) | −0.023 (12) | 0.003 (9) |
C24A | 0.103 (10) | 0.076 (10) | 0.078 (9) | 0.006 (8) | 0.020 (8) | 0.007 (7) |
Geometric parameters (Å, º) top
Co1—O3 | 1.854 (3) | C12—H12A | 0.9800 |
Co1—O2 | 1.891 (3) | C12—H12B | 0.9800 |
Co1—O1 | 1.907 (3) | C12—H12C | 0.9800 |
Co1—O4 | 1.884 (3) | C12—C11 | 1.531 (6) |
Co1—N1 | 1.954 (4) | C11—C14 | 1.534 (6) |
Co1—N2i | 1.964 (3) | C14—H14A | 0.9800 |
O3—C15 | 1.338 (5) | C14—H14B | 0.9800 |
O2—C2 | 1.316 (5) | C14—H14C | 0.9800 |
O1—C1 | 1.313 (4) | C29—H29 | 0.9500 |
O4—C16 | 1.356 (5) | C29—C31 | 1.376 (6) |
N1—C29 | 1.330 (6) | C35—H35A | 0.9900 |
N1—C30 | 1.330 (6) | C35—H35B | 0.9900 |
N2—Co1ii | 1.964 (3) | C35—C34 | 1.561 (7) |
N2—C41 | 1.338 (6) | C35—C36iii | 1.575 (6) |
N2—C40 | 1.348 (6) | C40—H40 | 0.9500 |
C4—H4 | 0.9500 | C40—C38 | 1.385 (6) |
C4—C3 | 1.368 (5) | C30—H30 | 0.9500 |
C4—C5 | 1.432 (5) | C30—C32 | 1.398 (7) |
C1—C2 | 1.440 (5) | C39—H39 | 0.9500 |
C1—C6 | 1.395 (5) | C39—C37 | 1.405 (9) |
C15—C16 | 1.408 (5) | C42—H42A | 0.9800 |
C15—C20 | 1.415 (5) | C42—H42B | 0.9800 |
C3—C2 | 1.438 (5) | C42—H42C | 0.9800 |
C3—C7 | 1.518 (5) | C42—C43 | 1.487 (9) |
C6—H6 | 0.9500 | C21—C24 | 1.537 (8) |
C6—C5 | 1.371 (5) | C21—C23 | 1.578 (10) |
O7—H7 | 0.8400 | C21—C22 | 1.551 (10) |
O7—C43 | 1.435 (7) | C21—C22A | 1.503 (18) |
C5—C11 | 1.528 (6) | C21—C23A | 1.51 (3) |
C16—C17 | 1.387 (6) | C21—C24A | 1.54 (2) |
C17—H17 | 0.9500 | C32—H32 | 0.9500 |
C17—C18 | 1.406 (6) | C32—C33 | 1.404 (9) |
C25—C20 | 1.538 (5) | C38—H38 | 0.9500 |
C25—C27 | 1.546 (6) | C38—C37 | 1.353 (9) |
C25—C28 | 1.523 (6) | C31—H31 | 0.9500 |
C25—C26 | 1.515 (6) | C31—C33 | 1.361 (9) |
C20—C19 | 1.406 (6) | C33—C34 | 1.538 (7) |
C19—H19 | 0.9500 | C37—C36 | 1.561 (7) |
C19—C18 | 1.397 (6) | C34—H34 | 1.0000 |
C27—H27A | 0.9800 | C34—C36 | 1.448 (6) |
C27—H27B | 0.9800 | C34—O6 | 1.451 (5) |
C27—H27C | 0.9800 | C36—C35iii | 1.575 (6) |
C8—H8A | 0.9800 | C36—H36 | 1.0000 |
C8—H8B | 0.9800 | C36—O5 | 1.451 (5) |
C8—H8C | 0.9800 | C43—H43A | 0.9900 |
C8—C7 | 1.550 (5) | C43—H43B | 0.9900 |
C28—H28A | 0.9800 | C24—H24A | 0.9800 |
C28—H28B | 0.9800 | C24—H24B | 0.9800 |
C28—H28C | 0.9800 | C24—H24C | 0.9800 |
C9—H9A | 0.9800 | C23—H23A | 0.9800 |
C9—H9B | 0.9800 | C23—H23B | 0.9800 |
C9—H9C | 0.9800 | C23—H23C | 0.9800 |
C9—C7 | 1.545 (6) | C22—H22A | 0.9800 |
C7—C10 | 1.535 (5) | C22—H22B | 0.9800 |
C26—H26A | 0.9800 | C22—H22C | 0.9800 |
C26—H26B | 0.9800 | O6—H6A | 0.8400 |
C26—H26C | 0.9800 | O5—H5 | 0.8400 |
C41—H41 | 0.9500 | C22A—H22D | 0.9800 |
C41—C39 | 1.386 (7) | C22A—H22E | 0.9800 |
C18—C21 | 1.518 (6) | C22A—H22F | 0.9800 |
C10—H10A | 0.9800 | C23A—H23D | 0.9800 |
C10—H10B | 0.9800 | C23A—H23E | 0.9800 |
C10—H10C | 0.9800 | C23A—H23F | 0.9800 |
C13—H13A | 0.9800 | C24A—H24D | 0.9800 |
C13—H13B | 0.9800 | C24A—H24E | 0.9800 |
C13—H13C | 0.9800 | C24A—H24F | 0.9800 |
C13—C11 | 1.541 (6) | | |
| | | |
O3—Co1—O2 | 87.65 (11) | C5—C11—C13 | 108.6 (4) |
O3—Co1—O1 | 87.03 (12) | C5—C11—C12 | 110.2 (3) |
O3—Co1—O4 | 87.95 (12) | C5—C11—C14 | 112.0 (3) |
O3—Co1—N1 | 87.73 (13) | C12—C11—C13 | 109.9 (4) |
O3—Co1—N2i | 178.92 (15) | C12—C11—C14 | 108.1 (4) |
O2—Co1—O1 | 85.28 (12) | C14—C11—C13 | 108.1 (4) |
O2—Co1—N1 | 174.63 (12) | C11—C14—H14A | 109.5 |
O2—Co1—N2i | 92.63 (13) | C11—C14—H14B | 109.5 |
O1—Co1—N1 | 91.75 (14) | C11—C14—H14C | 109.5 |
O1—Co1—N2i | 94.03 (14) | H14A—C14—H14B | 109.5 |
O4—Co1—O2 | 89.57 (12) | H14A—C14—H14C | 109.5 |
O4—Co1—O1 | 172.94 (12) | H14B—C14—H14C | 109.5 |
O4—Co1—N1 | 93.00 (15) | N1—C29—H29 | 118.3 |
O4—Co1—N2i | 91.01 (14) | N1—C29—C31 | 123.5 (5) |
N1—Co1—N2i | 92.04 (14) | C31—C29—H29 | 118.3 |
C15—O3—Co1 | 109.2 (2) | H35A—C35—H35B | 108.2 |
C2—O2—Co1 | 107.2 (2) | C34—C35—H35A | 109.8 |
C1—O1—Co1 | 106.4 (2) | C34—C35—H35B | 109.8 |
C16—O4—Co1 | 107.4 (2) | C34—C35—C36iii | 109.6 (4) |
C29—N1—Co1 | 122.6 (3) | C36iii—C35—H35A | 109.8 |
C29—N1—C30 | 117.9 (4) | C36iii—C35—H35B | 109.8 |
C30—N1—Co1 | 119.3 (3) | N2—C40—H40 | 118.3 |
C41—N2—Co1ii | 120.4 (3) | N2—C40—C38 | 123.4 (5) |
C41—N2—C40 | 117.5 (4) | C38—C40—H40 | 118.3 |
C40—N2—Co1ii | 122.0 (3) | N1—C30—H30 | 118.9 |
C3—C4—H4 | 117.6 | N1—C30—C32 | 122.2 (5) |
C3—C4—C5 | 124.7 (3) | C32—C30—H30 | 118.9 |
C5—C4—H4 | 117.6 | C41—C39—H39 | 120.0 |
O1—C1—C2 | 115.6 (3) | C41—C39—C37 | 120.1 (5) |
O1—C1—C6 | 124.0 (3) | C37—C39—H39 | 120.0 |
C6—C1—C2 | 120.4 (3) | H42A—C42—H42B | 109.5 |
O3—C15—C16 | 116.4 (3) | H42A—C42—H42C | 109.5 |
O3—C15—C20 | 123.3 (3) | H42B—C42—H42C | 109.5 |
C16—C15—C20 | 120.3 (4) | C43—C42—H42A | 109.5 |
C4—C3—C2 | 115.6 (3) | C43—C42—H42B | 109.5 |
C4—C3—C7 | 123.7 (3) | C43—C42—H42C | 109.5 |
C2—C3—C7 | 120.7 (3) | C18—C21—C24 | 110.0 (4) |
O2—C2—C1 | 115.5 (3) | C18—C21—C23 | 110.2 (5) |
O2—C2—C3 | 124.2 (3) | C18—C21—C22 | 115.0 (5) |
C3—C2—C1 | 120.3 (3) | C18—C21—C24A | 110.8 (9) |
C1—C6—H6 | 120.0 | C24—C21—C23 | 108.4 (5) |
C5—C6—C1 | 119.9 (4) | C24—C21—C22 | 106.7 (6) |
C5—C6—H6 | 120.0 | C22—C21—C23 | 106.2 (7) |
C43—O7—H7 | 109.5 | C22A—C21—C18 | 102.7 (8) |
C4—C5—C11 | 118.0 (3) | C22A—C21—C23A | 113.1 (11) |
C6—C5—C4 | 118.8 (4) | C22A—C21—C24A | 112.7 (12) |
C6—C5—C11 | 123.1 (4) | C23A—C21—C18 | 108.8 (9) |
O4—C16—C15 | 115.8 (4) | C23A—C21—C24A | 108.7 (13) |
O4—C16—C17 | 123.4 (4) | C30—C32—H32 | 120.5 |
C17—C16—C15 | 120.8 (4) | C30—C32—C33 | 119.0 (6) |
C16—C17—H17 | 119.8 | C33—C32—H32 | 120.5 |
C16—C17—C18 | 120.3 (4) | C40—C38—H38 | 120.3 |
C18—C17—H17 | 119.8 | C37—C38—C40 | 119.5 (6) |
C20—C25—C27 | 110.0 (3) | C37—C38—H38 | 120.3 |
C28—C25—C20 | 108.4 (3) | C29—C31—H31 | 120.1 |
C28—C25—C27 | 109.1 (3) | C33—C31—C29 | 119.9 (6) |
C26—C25—C20 | 112.4 (4) | C33—C31—H31 | 120.1 |
C26—C25—C27 | 108.4 (3) | C32—C33—C34 | 123.1 (6) |
C26—C25—C28 | 108.5 (3) | C31—C33—C32 | 117.6 (5) |
C15—C20—C25 | 120.2 (4) | C31—C33—C34 | 119.2 (6) |
C19—C20—C15 | 117.0 (4) | C39—C37—C36 | 124.4 (6) |
C19—C20—C25 | 122.7 (4) | C38—C37—C39 | 117.8 (5) |
C20—C19—H19 | 118.4 | C38—C37—C36 | 117.8 (6) |
C18—C19—C20 | 123.2 (4) | C35—C34—H34 | 109.4 |
C18—C19—H19 | 118.4 | C33—C34—C35 | 106.9 (4) |
C25—C27—H27A | 109.5 | C33—C34—H34 | 109.4 |
C25—C27—H27B | 109.5 | C36—C34—C35 | 108.4 (5) |
C25—C27—H27C | 109.5 | C36—C34—C33 | 113.3 (5) |
H27A—C27—H27B | 109.5 | C36—C34—H34 | 109.4 |
H27A—C27—H27C | 109.5 | C36—C34—O6 | 105.6 (8) |
H27B—C27—H27C | 109.5 | O6—C34—C35 | 109.7 (7) |
H8A—C8—H8B | 109.5 | O6—C34—C33 | 112.8 (7) |
H8A—C8—H8C | 109.5 | C35iii—C36—H36 | 110.1 |
H8B—C8—H8C | 109.5 | C37—C36—C35iii | 104.2 (4) |
C7—C8—H8A | 109.5 | C37—C36—H36 | 110.1 |
C7—C8—H8B | 109.5 | C34—C36—C35iii | 109.1 (4) |
C7—C8—H8C | 109.5 | C34—C36—C37 | 113.2 (5) |
C25—C28—H28A | 109.5 | C34—C36—H36 | 110.1 |
C25—C28—H28B | 109.5 | C34—C36—O5 | 105.6 (6) |
C25—C28—H28C | 109.5 | O5—C36—C35iii | 112.9 (6) |
H28A—C28—H28B | 109.5 | O5—C36—C37 | 112.0 (6) |
H28A—C28—H28C | 109.5 | O7—C43—C42 | 113.6 (5) |
H28B—C28—H28C | 109.5 | O7—C43—H43A | 108.8 |
H9A—C9—H9B | 109.5 | O7—C43—H43B | 108.8 |
H9A—C9—H9C | 109.5 | C42—C43—H43A | 108.8 |
H9B—C9—H9C | 109.5 | C42—C43—H43B | 108.8 |
C7—C9—H9A | 109.5 | H43A—C43—H43B | 107.7 |
C7—C9—H9B | 109.5 | C21—C24—H24A | 109.5 |
C7—C9—H9C | 109.5 | C21—C24—H24B | 109.5 |
C3—C7—C8 | 111.9 (3) | C21—C24—H24C | 109.5 |
C3—C7—C9 | 110.4 (3) | H24A—C24—H24B | 109.5 |
C3—C7—C10 | 109.1 (3) | H24A—C24—H24C | 109.5 |
C9—C7—C8 | 107.7 (3) | H24B—C24—H24C | 109.5 |
C10—C7—C8 | 107.2 (3) | C21—C23—H23A | 109.5 |
C10—C7—C9 | 110.5 (4) | C21—C23—H23B | 109.5 |
C25—C26—H26A | 109.5 | C21—C23—H23C | 109.5 |
C25—C26—H26B | 109.5 | H23A—C23—H23B | 109.5 |
C25—C26—H26C | 109.5 | H23A—C23—H23C | 109.5 |
H26A—C26—H26B | 109.5 | H23B—C23—H23C | 109.5 |
H26A—C26—H26C | 109.5 | C21—C22—H22A | 109.5 |
H26B—C26—H26C | 109.5 | C21—C22—H22B | 109.5 |
N2—C41—H41 | 119.2 | C21—C22—H22C | 109.5 |
N2—C41—C39 | 121.7 (5) | H22A—C22—H22B | 109.5 |
C39—C41—H41 | 119.2 | H22A—C22—H22C | 109.5 |
C17—C18—C21 | 119.9 (4) | H22B—C22—H22C | 109.5 |
C19—C18—C17 | 118.2 (4) | C34—O6—H6A | 109.5 |
C19—C18—C21 | 121.8 (4) | C36—O5—H5 | 109.5 |
C7—C10—H10A | 109.5 | C21—C22A—H22D | 109.5 |
C7—C10—H10B | 109.5 | C21—C22A—H22E | 109.5 |
C7—C10—H10C | 109.5 | C21—C22A—H22F | 109.5 |
H10A—C10—H10B | 109.5 | H22D—C22A—H22E | 109.5 |
H10A—C10—H10C | 109.5 | H22D—C22A—H22F | 109.5 |
H10B—C10—H10C | 109.5 | H22E—C22A—H22F | 109.5 |
H13A—C13—H13B | 109.5 | C21—C23A—H23D | 109.5 |
H13A—C13—H13C | 109.5 | C21—C23A—H23E | 109.5 |
H13B—C13—H13C | 109.5 | C21—C23A—H23F | 109.5 |
C11—C13—H13A | 109.5 | H23D—C23A—H23E | 109.5 |
C11—C13—H13B | 109.5 | H23D—C23A—H23F | 109.5 |
C11—C13—H13C | 109.5 | H23E—C23A—H23F | 109.5 |
H12A—C12—H12B | 109.5 | C21—C24A—H24D | 109.5 |
H12A—C12—H12C | 109.5 | C21—C24A—H24E | 109.5 |
H12B—C12—H12C | 109.5 | C21—C24A—H24F | 109.5 |
C11—C12—H12A | 109.5 | H24D—C24A—H24E | 109.5 |
C11—C12—H12B | 109.5 | H24D—C24A—H24F | 109.5 |
C11—C12—H12C | 109.5 | H24E—C24A—H24F | 109.5 |
| | | |
Co1—O3—C15—C16 | −8.5 (4) | C16—C17—C18—C19 | 2.3 (6) |
Co1—O3—C15—C20 | 173.2 (3) | C16—C17—C18—C21 | −175.9 (4) |
Co1—O2—C2—C1 | −20.7 (4) | C17—C18—C21—C24 | 62.3 (6) |
Co1—O2—C2—C3 | 159.4 (3) | C17—C18—C21—C23 | −57.3 (7) |
Co1—O1—C1—C2 | 22.9 (4) | C17—C18—C21—C22 | −177.3 (6) |
Co1—O1—C1—C6 | −157.2 (3) | C17—C18—C21—C22A | −114.7 (8) |
Co1—O4—C16—C15 | 15.4 (4) | C17—C18—C21—C23A | 125.3 (10) |
Co1—O4—C16—C17 | −166.9 (3) | C17—C18—C21—C24A | 5.9 (12) |
Co1—N1—C29—C31 | −174.2 (3) | C25—C20—C19—C18 | 178.0 (4) |
Co1—N1—C30—C32 | 174.5 (3) | C20—C15—C16—O4 | 173.3 (3) |
Co1ii—N2—C41—C39 | 178.6 (3) | C20—C15—C16—C17 | −4.5 (6) |
Co1ii—N2—C40—C38 | −178.1 (4) | C20—C19—C18—C17 | −1.7 (6) |
O3—Co1—O2—C2 | −60.5 (2) | C20—C19—C18—C21 | 176.5 (4) |
O3—Co1—O4—C16 | −16.2 (3) | C19—C18—C21—C24 | −115.8 (5) |
O3—C15—C16—O4 | −5.0 (5) | C19—C18—C21—C23 | 124.6 (6) |
O3—C15—C16—C17 | 177.2 (4) | C19—C18—C21—C22 | 4.7 (8) |
O3—C15—C20—C25 | 3.2 (6) | C19—C18—C21—C22A | 67.3 (9) |
O3—C15—C20—C19 | −176.9 (3) | C19—C18—C21—C23A | −52.8 (10) |
O2—Co1—O3—C15 | −75.8 (2) | C19—C18—C21—C24A | −172.2 (11) |
O2—Co1—O4—C16 | 71.5 (3) | C27—C25—C20—C15 | −59.3 (5) |
O1—Co1—O3—C15 | −161.2 (2) | C27—C25—C20—C19 | 120.8 (4) |
O1—Co1—O2—C2 | 26.7 (2) | C28—C25—C20—C15 | 60.0 (5) |
O1—C1—C2—O2 | −1.8 (5) | C28—C25—C20—C19 | −120.0 (4) |
O1—C1—C2—C3 | 178.2 (3) | C7—C3—C2—O2 | 1.4 (6) |
O1—C1—C6—C5 | 178.5 (4) | C7—C3—C2—C1 | −178.6 (3) |
O4—Co1—O3—C15 | 13.8 (2) | C26—C25—C20—C15 | 179.8 (4) |
O4—Co1—O2—C2 | −148.5 (2) | C26—C25—C20—C19 | −0.1 (5) |
O4—C16—C17—C18 | −176.9 (4) | C41—N2—C40—C38 | −1.5 (7) |
N1—Co1—O3—C15 | 106.9 (3) | C41—C39—C37—C38 | −1.6 (7) |
N1—Co1—O4—C16 | −103.8 (3) | C41—C39—C37—C36 | 175.2 (4) |
N1—C29—C31—C33 | −0.6 (7) | C29—N1—C30—C32 | −0.3 (7) |
N1—C30—C32—C33 | 0.3 (7) | C29—C31—C33—C32 | 0.6 (7) |
N2i—Co1—O2—C2 | 120.5 (3) | C29—C31—C33—C34 | −175.8 (4) |
N2i—Co1—O4—C16 | 164.1 (3) | C35—C34—C36—C35iii | −60.7 (7) |
N2—C41—C39—C37 | −0.4 (7) | C35—C34—C36—C37 | −176.2 (5) |
N2—C40—C38—C37 | −0.5 (8) | C35—C34—C36—O5 | 60.9 (7) |
C4—C3—C2—O2 | −176.8 (4) | C40—N2—C41—C39 | 1.9 (7) |
C4—C3—C2—C1 | 3.2 (5) | C40—C38—C37—C39 | 2.0 (8) |
C4—C3—C7—C8 | −3.5 (5) | C40—C38—C37—C36 | −175.0 (4) |
C4—C3—C7—C9 | 116.5 (4) | C30—N1—C29—C31 | 0.4 (7) |
C4—C3—C7—C10 | −121.9 (4) | C30—C32—C33—C31 | −0.5 (7) |
C4—C5—C11—C13 | −62.6 (5) | C30—C32—C33—C34 | 175.7 (4) |
C4—C5—C11—C12 | 57.8 (5) | C39—C37—C36—C35iii | −66.5 (6) |
C4—C5—C11—C14 | 178.1 (4) | C39—C37—C36—C34 | 51.8 (7) |
C1—C6—C5—C4 | 3.1 (6) | C39—C37—C36—O5 | 171.1 (7) |
C1—C6—C5—C11 | −176.6 (4) | C32—C33—C34—C35 | −61.1 (7) |
C15—C16—C17—C18 | 0.7 (6) | C32—C33—C34—C36 | 58.2 (7) |
C15—C20—C19—C18 | −1.9 (6) | C32—C33—C34—O6 | 178.1 (8) |
C3—C4—C5—C6 | −1.5 (6) | C38—C37—C36—C35iii | 110.3 (6) |
C3—C4—C5—C11 | 178.2 (4) | C38—C37—C36—C34 | −131.4 (6) |
C2—C1—C6—C5 | −1.5 (6) | C38—C37—C36—O5 | −12.1 (8) |
C2—C3—C7—C8 | 178.5 (3) | C31—C33—C34—C35 | 115.0 (6) |
C2—C3—C7—C9 | −61.5 (5) | C31—C33—C34—C36 | −125.6 (6) |
C2—C3—C7—C10 | 60.1 (5) | C31—C33—C34—O6 | −5.7 (9) |
C6—C1—C2—O2 | 178.3 (3) | C33—C34—C36—C35iii | −179.3 (5) |
C6—C1—C2—C3 | −1.7 (6) | C33—C34—C36—C37 | 65.3 (7) |
C6—C5—C11—C13 | 117.0 (4) | C33—C34—C36—O5 | −57.6 (7) |
C6—C5—C11—C12 | −122.5 (4) | C36iii—C35—C34—C33 | −176.4 (6) |
C6—C5—C11—C14 | −2.2 (6) | C36iii—C35—C34—C36 | 61.1 (7) |
C5—C4—C3—C2 | −1.7 (6) | C36iii—C35—C34—O6 | −53.8 (8) |
C5—C4—C3—C7 | −179.8 (4) | O6—C34—C36—C35iii | 56.8 (8) |
C16—C15—C20—C25 | −175.0 (4) | O6—C34—C36—C37 | −58.7 (8) |
C16—C15—C20—C19 | 4.9 (6) | | |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2; (iii) −x+1, −y+1, −z+1. |
catena-Poly[[[(3,5-di-
tert-butylbenzene-1,2-diolato)(1,5-di-
tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)cobalt(III)]-µ-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]–ethanol–water (1/1/5)] (2_100k)
top
Crystal data top
[Co(C14H20O2)2(C26H24N4O)]·C2H6O·5H2O | Z = 2 |
Mr = 1044.17 | F(000) = 1118 |
Triclinic, P1 | Dx = 1.240 Mg m−3 |
a = 10.072 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 16.135 (3) Å | Cell parameters from 60678 reflections |
c = 18.192 (4) Å | θ = 2.1–26.5° |
α = 75.34 (3)° | µ = 0.37 mm−1 |
β = 83.15 (3)° | T = 100 K |
γ = 78.70 (3)° | Plate, clear blue |
V = 2797.1 (11) Å3 | 0.1 × 0.04 × 0.02 mm |
Data collection top
ADSC Quantum 210r diffractometer | 17013 independent reflections |
Radiation source: MX1 Beamline Australian Synchrotron | 12047 reflections with I > 2σ(I) |
Silicon Double Crystal monochromator | Rint = 0.080 |
Phi Scan scans | θmax = 32.0°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2012) | h = −14→14 |
Tmin = 0.963, Tmax = 0.993 | k = −23→22 |
107853 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | Hydrogen site location: mixed |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.094 | w = 1/[σ2(Fo2) + (0.1327P)2 + 7.186P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.276 | (Δ/σ)max = 0.001 |
S = 1.04 | Δρmax = 2.65 e Å−3 |
17013 reflections | Δρmin = −0.85 e Å−3 |
682 parameters | Extinction correction: SHELXL-2018/3 (Sheldrick, 2018), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
88 restraints | Extinction coefficient: 0.067 (4) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Crystals were small and weakly scattering, hence data collection was carried
out at the Australian Synchrotron. Some of the crystals were disordered, the
crystals showed minor disorder, however the Rint value was still relatively
high. During the refinement it was found the structure was disordered: the
alcohol group of the tpch ligand is disordered over four positions on the
cyclohexane ring and so refinement was carried out with these atoms restrained
to ideal geometry. One of the tert-butyl groups also displays disorder and so
refinement was carried out with these groups disordered over two components,
both being restrained to ideal geometry. The maximum residual electron
density peaks, 2.645 eA-3, were close one of the pydidyl groups of the tpch
ligand indicating that this group was somewhat disordered. Attempts to model
this disorder were not successful. The disorder required a number of distance
and angle constraints and restraints to ensure the disordered components were
maintained at a chemical reasonable geometry. The displacement parameters of
each of the atoms of each component were constrained to be equal. The crystal
showed a solvent void containing disordered/diffuse solvent consistent with 5
molecules of water per formula unit (containing one cobalt atom). There were
seven reflections OMITted due to anomalous background. The high final R and
wR values are a consequence of the disorder of the crystals. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.37965 (4) | 0.57434 (3) | 0.77409 (2) | 0.02219 (14) | |
O1 | 0.2329 (2) | 0.57475 (15) | 0.72056 (14) | 0.0276 (5) | |
O2 | 0.2626 (2) | 0.64608 (15) | 0.82992 (14) | 0.0282 (5) | |
O3 | 0.4869 (2) | 0.49651 (14) | 0.71821 (13) | 0.0251 (5) | |
O4 | 0.3433 (3) | 0.47224 (15) | 0.84861 (14) | 0.0311 (5) | |
N1 | 0.4205 (3) | 0.67522 (16) | 0.69664 (15) | 0.0229 (5) | |
N2 | 0.9848 (3) | 1.12061 (19) | 0.5259 (2) | 0.0361 (7) | |
N3 | 0.5368 (3) | 0.57308 (17) | 0.82811 (16) | 0.0264 (5) | |
C1 | 0.1454 (3) | 0.6732 (2) | 0.79613 (19) | 0.0257 (6) | |
C2 | 0.1283 (3) | 0.6349 (2) | 0.73630 (19) | 0.0254 (6) | |
C3 | 0.0093 (4) | 0.6614 (2) | 0.6969 (2) | 0.0286 (7) | |
C4 | −0.0907 (4) | 0.7249 (2) | 0.7210 (2) | 0.0317 (7) | |
H4 | −0.172112 | 0.743386 | 0.695451 | 0.038* | |
C5 | −0.0770 (4) | 0.7630 (2) | 0.7814 (2) | 0.0328 (7) | |
C6 | 0.0430 (4) | 0.7362 (2) | 0.8180 (2) | 0.0290 (7) | |
H6 | 0.055399 | 0.761010 | 0.858340 | 0.035* | |
C7 | −0.1918 (4) | 0.8314 (3) | 0.8045 (3) | 0.0423 (9) | |
C8 | −0.1593 (6) | 0.8629 (4) | 0.8727 (3) | 0.0611 (14) | |
H8A | −0.141820 | 0.813093 | 0.916290 | 0.092* | |
H8B | −0.236641 | 0.904851 | 0.886499 | 0.092* | |
H8C | −0.078761 | 0.890773 | 0.858671 | 0.092* | |
C9 | −0.3205 (5) | 0.7893 (4) | 0.8322 (3) | 0.0603 (13) | |
H9A | −0.345559 | 0.766683 | 0.791613 | 0.090* | |
H9B | −0.395480 | 0.833197 | 0.845314 | 0.090* | |
H9C | −0.301773 | 0.741636 | 0.877264 | 0.090* | |
C10 | −0.2247 (7) | 0.9065 (4) | 0.7387 (3) | 0.0717 (18) | |
H10A | −0.145303 | 0.935052 | 0.721792 | 0.108* | |
H10B | −0.300905 | 0.948046 | 0.754202 | 0.108* | |
H10C | −0.249556 | 0.885878 | 0.696825 | 0.108* | |
C11 | −0.0047 (4) | 0.6234 (2) | 0.6296 (2) | 0.0333 (7) | |
C12 | 0.0084 (4) | 0.5230 (3) | 0.6554 (2) | 0.0390 (8) | |
H12A | 0.005921 | 0.499318 | 0.611038 | 0.058* | |
H12B | −0.066993 | 0.507904 | 0.692539 | 0.058* | |
H12C | 0.094656 | 0.498257 | 0.678721 | 0.058* | |
C13 | 0.1082 (4) | 0.6438 (3) | 0.5672 (2) | 0.0384 (8) | |
H13A | 0.103973 | 0.706956 | 0.550637 | 0.058* | |
H13B | 0.096416 | 0.621019 | 0.523755 | 0.058* | |
H13C | 0.196621 | 0.616621 | 0.587130 | 0.058* | |
C14 | −0.1429 (4) | 0.6598 (3) | 0.5954 (3) | 0.0468 (10) | |
H14A | −0.155940 | 0.723433 | 0.581201 | 0.070* | |
H14B | −0.215605 | 0.641055 | 0.633075 | 0.070* | |
H14C | −0.145015 | 0.637907 | 0.549988 | 0.070* | |
C15 | 0.4044 (3) | 0.4027 (2) | 0.82641 (19) | 0.0268 (6) | |
C16 | 0.4819 (3) | 0.41566 (19) | 0.75339 (18) | 0.0235 (6) | |
C17 | 0.5484 (3) | 0.34293 (19) | 0.72401 (19) | 0.0250 (6) | |
C18 | 0.5360 (4) | 0.2612 (2) | 0.7695 (2) | 0.0315 (7) | |
H18 | 0.579375 | 0.211732 | 0.751097 | 0.038* | |
C19 | 0.4625 (4) | 0.2471 (2) | 0.8417 (2) | 0.0387 (9) | |
C20 | 0.3968 (4) | 0.3178 (2) | 0.8693 (2) | 0.0356 (8) | |
H20 | 0.346342 | 0.309044 | 0.917411 | 0.043* | |
C21 | 0.6281 (4) | 0.3563 (2) | 0.6462 (2) | 0.0292 (7) | |
C22 | 0.7456 (4) | 0.4042 (3) | 0.6474 (3) | 0.0406 (9) | |
H22A | 0.708721 | 0.461651 | 0.657141 | 0.061* | |
H22B | 0.798446 | 0.411106 | 0.598038 | 0.061* | |
H22C | 0.804349 | 0.370436 | 0.687706 | 0.061* | |
C23 | 0.5359 (5) | 0.4088 (3) | 0.5842 (2) | 0.0441 (10) | |
H23A | 0.464103 | 0.376595 | 0.581768 | 0.066* | |
H23B | 0.589209 | 0.418735 | 0.534994 | 0.066* | |
H23C | 0.494999 | 0.464796 | 0.595693 | 0.066* | |
C24 | 0.6903 (5) | 0.2690 (2) | 0.6258 (2) | 0.0397 (9) | |
H24A | 0.750136 | 0.233668 | 0.665112 | 0.060* | |
H24B | 0.742754 | 0.279932 | 0.576463 | 0.060* | |
H24C | 0.617477 | 0.237776 | 0.622982 | 0.060* | |
C25 | 0.4568 (5) | 0.1535 (2) | 0.8887 (3) | 0.0607 (15) | |
C29 | 0.4429 (3) | 0.67320 (19) | 0.62257 (18) | 0.0238 (6) | |
H29 | 0.440307 | 0.620794 | 0.608415 | 0.029* | |
C30 | 0.4236 (4) | 0.7506 (2) | 0.7150 (2) | 0.0310 (7) | |
H30 | 0.407133 | 0.753096 | 0.766997 | 0.037* | |
C31 | 0.4497 (4) | 0.8246 (2) | 0.6614 (2) | 0.0329 (8) | |
H31 | 0.451999 | 0.876216 | 0.677011 | 0.039* | |
C32 | 0.4697 (3) | 0.7454 (2) | 0.56618 (19) | 0.0256 (6) | |
H32 | 0.486235 | 0.741350 | 0.514573 | 0.031* | |
C33 | 0.4723 (3) | 0.82349 (19) | 0.58496 (19) | 0.0260 (6) | |
C34 | 0.4949 (3) | 0.90446 (19) | 0.52309 (18) | 0.0270 (6) | 0.696 (3) |
H34 | 0.516186 | 0.888774 | 0.472689 | 0.032* | 0.696 (3) |
C36 | 0.6125 (4) | 0.9424 (2) | 0.5406 (2) | 0.0288 (7) | 0.5 |
H36A | 0.696204 | 0.898172 | 0.543034 | 0.035* | 0.5 |
H36B | 0.592011 | 0.956419 | 0.591166 | 0.035* | 0.5 |
C37 | 0.6372 (4) | 1.0254 (2) | 0.4800 (2) | 0.0286 (7) | 0.196 (3) |
O6 | 0.6495 (15) | 0.9994 (7) | 0.4085 (4) | 0.036 (3) | 0.196 (3) |
H6A | 0.731229 | 0.980037 | 0.397665 | 0.054* | 0.196 (3) |
C34A | 0.4949 (3) | 0.90446 (19) | 0.52309 (18) | 0.0270 (6) | 0.304 (3) |
O6A | 0.5281 (7) | 0.8821 (4) | 0.4499 (2) | 0.0232 (15) | 0.304 (3) |
H6AA | 0.589254 | 0.837860 | 0.454261 | 0.035* | 0.304 (3) |
C36A | 0.6125 (4) | 0.9424 (2) | 0.5406 (2) | 0.0288 (7) | 0.5 |
H36C | 0.696204 | 0.898172 | 0.543034 | 0.035* | 0.5 |
H36D | 0.592011 | 0.956419 | 0.591166 | 0.035* | 0.5 |
C37A | 0.6372 (4) | 1.0254 (2) | 0.4800 (2) | 0.0286 (7) | 0.804 (3) |
H37A | 0.657154 | 1.010536 | 0.429247 | 0.034* | 0.804 (3) |
C38 | 0.7576 (4) | 1.0599 (2) | 0.4967 (2) | 0.0290 (7) | |
C39 | 0.7749 (4) | 1.0688 (2) | 0.5694 (2) | 0.0306 (7) | |
H39 | 0.708477 | 1.055286 | 0.610218 | 0.037* | |
C40 | 0.8900 (4) | 1.0975 (2) | 0.5814 (2) | 0.0349 (8) | |
H40 | 0.902000 | 1.100865 | 0.631491 | 0.042* | |
C41 | 0.9676 (4) | 1.1144 (2) | 0.4559 (2) | 0.0374 (8) | |
H41 | 1.033923 | 1.130944 | 0.415906 | 0.045* | |
C42 | 0.8571 (4) | 1.0850 (2) | 0.4393 (2) | 0.0328 (7) | |
H42 | 0.848889 | 1.081757 | 0.388645 | 0.039* | |
C43 | 0.5282 (4) | 0.5733 (2) | 0.9023 (2) | 0.0355 (8) | |
H43 | 0.440 (7) | 0.584 (4) | 0.921 (4) | 0.08 (2)* | |
C44 | 0.6424 (5) | 0.5598 (3) | 0.9423 (3) | 0.0474 (11) | |
H44 | 0.623 (5) | 0.548 (3) | 0.999 (3) | 0.039 (12)* | |
C45 | 0.6619 (4) | 0.5637 (3) | 0.7920 (2) | 0.0357 (8) | |
H45 | 0.669 (5) | 0.559 (3) | 0.740 (3) | 0.049 (14)* | |
C46 | 0.7790 (4) | 0.5509 (3) | 0.8276 (3) | 0.0504 (11) | |
H46 | 0.864811 | 0.544804 | 0.799606 | 0.060* | |
C47 | 0.7708 (5) | 0.5470 (3) | 0.9048 (3) | 0.0553 (13) | |
C48 | 0.9116 (5) | 0.5311 (4) | 0.9359 (3) | 0.0564 (12) | 0.780 (3) |
H48 | 0.979718 | 0.546750 | 0.892328 | 0.068* | 0.780 (3) |
C49 | 0.9127 (4) | 0.5859 (2) | 0.9917 (2) | 0.0353 (8) | 0.5 |
H49A | 0.839985 | 0.574534 | 1.032719 | 0.042* | 0.5 |
H49B | 0.893478 | 0.648148 | 0.965227 | 0.042* | 0.5 |
C50 | 0.9467 (5) | 0.4340 (4) | 0.9720 (3) | 0.0576 (12) | 0.280 (3) |
O5 | 0.8271 (8) | 0.4176 (12) | 1.0225 (6) | 0.079 (6) | 0.280 (3) |
H5 | 0.806348 | 0.455489 | 1.048132 | 0.119* | 0.280 (3) |
C48A | 0.9116 (5) | 0.5311 (4) | 0.9359 (3) | 0.0564 (12) | 0.220 (3) |
O5A | 1.0270 (11) | 0.5183 (14) | 0.8816 (8) | 0.093 (8) | 0.220 (3) |
H5A | 1.027672 | 0.563996 | 0.847018 | 0.139* | 0.220 (3) |
C49A | 0.9127 (4) | 0.5859 (2) | 0.9917 (2) | 0.0353 (8) | 0.5 |
H49C | 0.839985 | 0.574534 | 1.032719 | 0.042* | 0.5 |
H49D | 0.893478 | 0.648148 | 0.965227 | 0.042* | 0.5 |
C50A | 0.9467 (5) | 0.4340 (4) | 0.9720 (3) | 0.0576 (12) | 0.720 (3) |
H50A | 0.876213 | 0.419748 | 1.014586 | 0.069* | 0.720 (3) |
C51 | 0.9490 (4) | 0.3750 (2) | 0.9209 (2) | 0.0468 (10) | |
C53 | 0.8528 (4) | 0.3206 (3) | 0.9372 (3) | 0.111 (3) | |
H53 | 0.789970 | 0.320956 | 0.980445 | 0.133* | |
C55 | 0.8485 (5) | 0.2656 (3) | 0.8901 (4) | 0.174 (5) | |
H55 | 0.782664 | 0.228401 | 0.901147 | 0.208* | |
N4 | 0.9404 (6) | 0.2650 (3) | 0.8267 (3) | 0.134 (3) | |
C54 | 1.0366 (5) | 0.3195 (3) | 0.8105 (2) | 0.103 (3) | |
H54 | 1.099441 | 0.319072 | 0.767203 | 0.123* | |
C52 | 1.0410 (3) | 0.3744 (3) | 0.8576 (2) | 0.0742 (19) | |
H52 | 1.106750 | 0.411628 | 0.846500 | 0.089* | |
C26 | 0.5214 (11) | 0.1470 (6) | 0.9684 (4) | 0.061 (3) | 0.5 |
H26A | 0.616372 | 0.154866 | 0.957939 | 0.091* | 0.5 |
H26B | 0.516540 | 0.089707 | 1.002453 | 0.091* | 0.5 |
H26C | 0.469969 | 0.192354 | 0.992670 | 0.091* | 0.5 |
C27 | 0.5427 (10) | 0.0834 (4) | 0.8566 (5) | 0.058 (3) | 0.5 |
H27A | 0.513353 | 0.085845 | 0.806570 | 0.086* | 0.5 |
H27B | 0.533855 | 0.026827 | 0.890880 | 0.086* | 0.5 |
H27C | 0.637757 | 0.091229 | 0.851289 | 0.086* | 0.5 |
C28 | 0.3131 (7) | 0.1412 (5) | 0.9125 (6) | 0.051 (2) | 0.5 |
H28A | 0.264481 | 0.190021 | 0.933403 | 0.076* | 0.5 |
H28B | 0.312216 | 0.086774 | 0.951490 | 0.076* | 0.5 |
H28C | 0.268519 | 0.138766 | 0.868267 | 0.076* | 0.5 |
C0AA | 0.5961 (8) | 0.1027 (6) | 0.8997 (7) | 0.071 (3) | 0.5 |
H0AA | 0.644535 | 0.100849 | 0.849988 | 0.107* | 0.5 |
H0AB | 0.590392 | 0.043303 | 0.928993 | 0.107* | 0.5 |
H0AC | 0.645196 | 0.130384 | 0.927534 | 0.107* | 0.5 |
C1AA | 0.3596 (11) | 0.1465 (7) | 0.9560 (6) | 0.073 (4) | 0.5 |
H1AA | 0.379912 | 0.180945 | 0.989261 | 0.110* | 0.5 |
H1AB | 0.366686 | 0.085460 | 0.983866 | 0.110* | 0.5 |
H1AC | 0.267207 | 0.168462 | 0.939871 | 0.110* | 0.5 |
C2AA | 0.3960 (15) | 0.1147 (9) | 0.8290 (6) | 0.107 (6) | 0.5 |
H2AA | 0.303330 | 0.145350 | 0.819599 | 0.160* | 0.5 |
H2AB | 0.394888 | 0.052560 | 0.850159 | 0.160* | 0.5 |
H2AC | 0.452939 | 0.122444 | 0.780994 | 0.160* | 0.5 |
O7 | 1.1954 (4) | 1.1587 (3) | 0.5891 (3) | 0.0783 (14) | |
H7 | 1.133791 | 1.142218 | 0.571960 | 0.118* | |
C01L | 1.1381 (7) | 1.2333 (5) | 0.6198 (4) | 0.0748 (17) | |
H01A | 1.086957 | 1.214753 | 0.669345 | 0.090* | |
H01B | 1.074670 | 1.274722 | 0.584483 | 0.090* | |
C01U | 1.2478 (11) | 1.2749 (10) | 0.6298 (8) | 0.165 (6) | |
H01C | 1.305830 | 1.285293 | 0.582364 | 0.247* | |
H01D | 1.301677 | 1.237041 | 0.670843 | 0.247* | |
H01E | 1.209936 | 1.330458 | 0.643081 | 0.247* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0249 (2) | 0.0139 (2) | 0.0232 (2) | −0.00038 (14) | −0.00043 (15) | 0.00102 (14) |
O1 | 0.0284 (11) | 0.0226 (11) | 0.0307 (12) | −0.0036 (9) | 0.0011 (9) | −0.0065 (9) |
O2 | 0.0267 (11) | 0.0260 (11) | 0.0298 (12) | −0.0013 (9) | −0.0014 (9) | −0.0057 (9) |
O3 | 0.0306 (11) | 0.0169 (10) | 0.0234 (10) | −0.0021 (8) | 0.0031 (9) | −0.0008 (8) |
O4 | 0.0364 (13) | 0.0214 (11) | 0.0290 (12) | −0.0021 (9) | 0.0084 (10) | −0.0011 (9) |
N1 | 0.0264 (13) | 0.0150 (11) | 0.0239 (12) | −0.0014 (9) | −0.0042 (10) | 0.0008 (9) |
N2 | 0.0347 (16) | 0.0221 (13) | 0.0490 (19) | −0.0003 (11) | −0.0063 (14) | −0.0060 (12) |
N3 | 0.0275 (13) | 0.0201 (12) | 0.0263 (13) | 0.0017 (10) | −0.0015 (11) | −0.0004 (10) |
C1 | 0.0252 (14) | 0.0187 (13) | 0.0301 (15) | −0.0026 (11) | −0.0003 (12) | −0.0016 (11) |
C2 | 0.0259 (15) | 0.0214 (14) | 0.0264 (15) | −0.0055 (11) | 0.0050 (12) | −0.0030 (11) |
C3 | 0.0289 (16) | 0.0226 (14) | 0.0332 (17) | −0.0061 (12) | 0.0016 (13) | −0.0050 (12) |
C4 | 0.0262 (16) | 0.0305 (16) | 0.0374 (18) | −0.0006 (13) | −0.0040 (14) | −0.0088 (14) |
C5 | 0.0297 (17) | 0.0234 (15) | 0.043 (2) | 0.0000 (12) | −0.0029 (15) | −0.0081 (14) |
C6 | 0.0299 (16) | 0.0207 (14) | 0.0346 (17) | −0.0019 (12) | −0.0007 (13) | −0.0058 (12) |
C7 | 0.037 (2) | 0.037 (2) | 0.051 (2) | 0.0124 (16) | −0.0110 (18) | −0.0189 (18) |
C8 | 0.065 (3) | 0.057 (3) | 0.054 (3) | 0.024 (2) | −0.005 (2) | −0.025 (2) |
C9 | 0.042 (2) | 0.069 (3) | 0.067 (3) | 0.005 (2) | 0.006 (2) | −0.027 (3) |
C10 | 0.085 (4) | 0.049 (3) | 0.059 (3) | 0.028 (3) | 0.002 (3) | −0.007 (2) |
C11 | 0.0321 (17) | 0.0331 (17) | 0.0357 (18) | −0.0069 (14) | −0.0010 (14) | −0.0095 (14) |
C12 | 0.041 (2) | 0.0370 (19) | 0.044 (2) | −0.0139 (16) | 0.0005 (17) | −0.0159 (16) |
C13 | 0.042 (2) | 0.040 (2) | 0.0319 (18) | −0.0075 (16) | 0.0012 (15) | −0.0067 (15) |
C14 | 0.036 (2) | 0.061 (3) | 0.047 (2) | −0.0013 (19) | −0.0092 (18) | −0.021 (2) |
C15 | 0.0287 (15) | 0.0176 (13) | 0.0282 (15) | 0.0003 (11) | 0.0014 (12) | 0.0004 (11) |
C16 | 0.0242 (14) | 0.0162 (12) | 0.0261 (14) | 0.0003 (10) | −0.0014 (11) | −0.0008 (10) |
C17 | 0.0264 (14) | 0.0163 (13) | 0.0290 (15) | −0.0004 (11) | −0.0024 (12) | −0.0018 (11) |
C18 | 0.0340 (17) | 0.0170 (14) | 0.0372 (18) | −0.0013 (12) | 0.0009 (14) | 0.0008 (12) |
C19 | 0.048 (2) | 0.0171 (14) | 0.0392 (19) | −0.0011 (14) | 0.0104 (17) | 0.0044 (13) |
C20 | 0.0395 (19) | 0.0221 (15) | 0.0337 (18) | −0.0014 (13) | 0.0116 (15) | 0.0047 (13) |
C21 | 0.0363 (17) | 0.0204 (14) | 0.0284 (16) | −0.0029 (12) | 0.0004 (13) | −0.0039 (12) |
C22 | 0.037 (2) | 0.041 (2) | 0.045 (2) | −0.0139 (16) | 0.0154 (17) | −0.0175 (17) |
C23 | 0.065 (3) | 0.0324 (19) | 0.0326 (19) | 0.0004 (18) | −0.0118 (19) | −0.0069 (15) |
C24 | 0.052 (2) | 0.0268 (17) | 0.0370 (19) | −0.0031 (16) | 0.0055 (17) | −0.0083 (14) |
C25 | 0.068 (3) | 0.0179 (17) | 0.075 (3) | −0.0023 (18) | 0.023 (3) | 0.0097 (19) |
C29 | 0.0269 (14) | 0.0169 (12) | 0.0251 (14) | −0.0011 (11) | −0.0032 (12) | −0.0018 (10) |
C30 | 0.046 (2) | 0.0176 (14) | 0.0281 (16) | −0.0056 (13) | −0.0055 (14) | −0.0012 (11) |
C31 | 0.053 (2) | 0.0154 (13) | 0.0292 (16) | −0.0084 (13) | −0.0024 (15) | −0.0009 (11) |
C32 | 0.0280 (15) | 0.0194 (13) | 0.0258 (15) | −0.0019 (11) | −0.0054 (12) | 0.0010 (11) |
C33 | 0.0299 (15) | 0.0152 (13) | 0.0286 (15) | 0.0004 (11) | −0.0047 (12) | 0.0006 (11) |
C34 | 0.0316 (16) | 0.0154 (13) | 0.0287 (15) | −0.0018 (11) | −0.0035 (13) | 0.0031 (11) |
C36 | 0.0314 (16) | 0.0160 (13) | 0.0332 (17) | −0.0018 (11) | −0.0033 (13) | 0.0032 (11) |
C37 | 0.0317 (16) | 0.0168 (13) | 0.0319 (16) | −0.0011 (11) | −0.0018 (13) | 0.0016 (11) |
O6 | 0.043 (7) | 0.022 (6) | 0.036 (7) | −0.007 (5) | 0.000 (6) | 0.005 (5) |
C34A | 0.0316 (16) | 0.0154 (13) | 0.0287 (15) | −0.0018 (11) | −0.0035 (13) | 0.0031 (11) |
O6A | 0.022 (3) | 0.014 (3) | 0.027 (3) | 0.001 (2) | 0.002 (3) | 0.003 (2) |
C36A | 0.0314 (16) | 0.0160 (13) | 0.0332 (17) | −0.0018 (11) | −0.0033 (13) | 0.0032 (11) |
C37A | 0.0317 (16) | 0.0168 (13) | 0.0319 (16) | −0.0011 (11) | −0.0018 (13) | 0.0016 (11) |
C38 | 0.0308 (16) | 0.0166 (13) | 0.0338 (17) | 0.0004 (11) | −0.0025 (13) | 0.0012 (12) |
C39 | 0.0381 (18) | 0.0188 (14) | 0.0300 (16) | 0.0001 (12) | −0.0011 (14) | −0.0013 (12) |
C40 | 0.0392 (19) | 0.0205 (15) | 0.042 (2) | 0.0037 (13) | −0.0082 (16) | −0.0061 (13) |
C41 | 0.0365 (19) | 0.0249 (16) | 0.046 (2) | −0.0037 (14) | 0.0031 (16) | −0.0039 (15) |
C42 | 0.0359 (18) | 0.0221 (15) | 0.0352 (18) | −0.0026 (13) | 0.0006 (14) | −0.0011 (13) |
C43 | 0.043 (2) | 0.0309 (17) | 0.0274 (17) | 0.0010 (15) | −0.0053 (15) | −0.0024 (13) |
C44 | 0.062 (3) | 0.038 (2) | 0.040 (2) | 0.0081 (19) | −0.022 (2) | −0.0109 (17) |
C45 | 0.0291 (17) | 0.0364 (19) | 0.041 (2) | 0.0002 (14) | −0.0045 (15) | −0.0109 (15) |
C46 | 0.031 (2) | 0.058 (3) | 0.066 (3) | 0.0111 (18) | −0.015 (2) | −0.031 (2) |
C47 | 0.048 (2) | 0.051 (3) | 0.073 (3) | 0.023 (2) | −0.035 (2) | −0.035 (2) |
C48 | 0.053 (3) | 0.059 (3) | 0.055 (3) | 0.002 (2) | −0.015 (2) | −0.014 (2) |
C49 | 0.0367 (19) | 0.0313 (17) | 0.0323 (18) | 0.0061 (14) | −0.0065 (15) | −0.0046 (14) |
C50 | 0.0579 (15) | 0.0569 (15) | 0.0573 (15) | −0.0074 (9) | −0.0074 (9) | −0.0127 (9) |
O5 | 0.031 (6) | 0.133 (14) | 0.040 (6) | −0.009 (7) | −0.004 (5) | 0.036 (8) |
C48A | 0.053 (3) | 0.059 (3) | 0.055 (3) | 0.002 (2) | −0.015 (2) | −0.014 (2) |
O5A | 0.090 (14) | 0.17 (2) | 0.038 (8) | −0.095 (16) | −0.008 (9) | 0.005 (11) |
C49A | 0.0367 (19) | 0.0313 (17) | 0.0323 (18) | 0.0061 (14) | −0.0065 (15) | −0.0046 (14) |
C50A | 0.0579 (15) | 0.0569 (15) | 0.0573 (15) | −0.0074 (9) | −0.0074 (9) | −0.0127 (9) |
C51 | 0.044 (2) | 0.039 (2) | 0.057 (3) | −0.0016 (17) | −0.020 (2) | −0.0065 (19) |
C53 | 0.114 (5) | 0.088 (4) | 0.139 (5) | −0.037 (4) | 0.008 (4) | −0.032 (4) |
C55 | 0.178 (7) | 0.177 (7) | 0.184 (7) | −0.053 (5) | −0.017 (5) | −0.058 (5) |
N4 | 0.156 (5) | 0.114 (4) | 0.146 (5) | −0.021 (4) | −0.019 (4) | −0.055 (4) |
C54 | 0.105 (4) | 0.108 (4) | 0.095 (4) | 0.006 (4) | −0.022 (3) | −0.035 (4) |
C52 | 0.060 (3) | 0.104 (5) | 0.055 (3) | 0.022 (3) | −0.026 (3) | −0.029 (3) |
C26 | 0.086 (8) | 0.033 (4) | 0.046 (5) | −0.001 (4) | −0.010 (5) | 0.016 (4) |
C27 | 0.069 (6) | 0.018 (3) | 0.064 (6) | 0.003 (4) | 0.019 (5) | 0.010 (3) |
C28 | 0.058 (5) | 0.018 (3) | 0.063 (6) | −0.010 (3) | 0.022 (5) | 0.007 (4) |
C0AA | 0.075 (7) | 0.028 (4) | 0.081 (8) | 0.009 (4) | −0.001 (6) | 0.025 (5) |
C1AA | 0.088 (9) | 0.036 (5) | 0.075 (8) | −0.014 (5) | 0.024 (7) | 0.012 (5) |
C2AA | 0.141 (13) | 0.068 (8) | 0.097 (10) | −0.044 (9) | 0.009 (9) | 0.018 (7) |
O7 | 0.045 (2) | 0.087 (3) | 0.124 (4) | −0.004 (2) | −0.012 (2) | −0.065 (3) |
C01L | 0.079 (4) | 0.083 (4) | 0.070 (4) | −0.022 (3) | −0.006 (3) | −0.026 (3) |
C01U | 0.089 (6) | 0.238 (15) | 0.236 (14) | −0.066 (8) | 0.012 (8) | −0.163 (13) |
Geometric parameters (Å, º) top
Co1—O1 | 1.863 (3) | C34—C36 | 1.534 (5) |
Co1—O2 | 1.880 (3) | C34—C37i | 1.565 (5) |
Co1—O3 | 1.905 (2) | C36—H36A | 0.9900 |
Co1—O4 | 1.917 (2) | C36—H36B | 0.9900 |
Co1—N1 | 1.941 (3) | C36—C37 | 1.546 (4) |
Co1—N3 | 1.955 (3) | C37—O6 | 1.4504 (11) |
O1—C2 | 1.343 (4) | C37—C38 | 1.519 (5) |
O2—C1 | 1.341 (4) | O6—H6A | 0.8400 |
O3—C16 | 1.307 (4) | C34A—O6A | 1.4508 (11) |
O4—C15 | 1.305 (4) | C34A—C36A | 1.534 (5) |
N1—C29 | 1.347 (4) | O6A—H6AA | 0.8400 |
N1—C30 | 1.347 (4) | C36A—H36C | 0.9900 |
N2—C40 | 1.337 (5) | C36A—H36D | 0.9900 |
N2—C41 | 1.336 (6) | C36A—C37A | 1.546 (4) |
N3—C43 | 1.342 (5) | C37A—H37A | 1.0000 |
N3—C45 | 1.349 (5) | C37A—C38 | 1.519 (5) |
C1—C2 | 1.423 (5) | C38—C39 | 1.402 (5) |
C1—C6 | 1.397 (5) | C38—C42 | 1.398 (5) |
C2—C3 | 1.408 (5) | C39—H39 | 0.9500 |
C3—C4 | 1.405 (5) | C39—C40 | 1.388 (5) |
C3—C11 | 1.533 (5) | C40—H40 | 0.9500 |
C4—H4 | 0.9500 | C41—H41 | 0.9500 |
C4—C5 | 1.419 (5) | C41—C42 | 1.384 (6) |
C5—C6 | 1.391 (5) | C42—H42 | 0.9500 |
C5—C7 | 1.533 (5) | C43—H43 | 0.91 (7) |
C6—H6 | 0.9500 | C43—C44 | 1.387 (6) |
C7—C8 | 1.547 (7) | C44—H44 | 1.00 (5) |
C7—C9 | 1.552 (7) | C44—C47 | 1.393 (8) |
C7—C10 | 1.488 (7) | C45—H45 | 0.97 (5) |
C8—H8A | 0.9800 | C45—C46 | 1.367 (6) |
C8—H8B | 0.9800 | C46—H46 | 0.9500 |
C8—H8C | 0.9800 | C46—C47 | 1.383 (7) |
C9—H9A | 0.9800 | C47—C48 | 1.540 (7) |
C9—H9B | 0.9800 | C47—C48A | 1.540 (7) |
C9—H9C | 0.9800 | C48—H48 | 1.0000 |
C10—H10A | 0.9800 | C48—C49 | 1.508 (7) |
C10—H10B | 0.9800 | C48—C50 | 1.526 (8) |
C10—H10C | 0.9800 | C49—H49A | 0.9900 |
C11—C12 | 1.552 (5) | C49—H49B | 0.9900 |
C11—C13 | 1.530 (5) | C49—C50ii | 1.575 (7) |
C11—C14 | 1.540 (6) | C50—O5 | 1.4505 (11) |
C12—H12A | 0.9800 | C50—C51 | 1.484 (6) |
C12—H12B | 0.9800 | O5—H5 | 0.8400 |
C12—H12C | 0.9800 | C48A—O5A | 1.4504 (11) |
C13—H13A | 0.9800 | C48A—C49A | 1.508 (7) |
C13—H13B | 0.9800 | C48A—C50A | 1.526 (8) |
C13—H13C | 0.9800 | O5A—H5A | 0.8400 |
C14—H14A | 0.9800 | C49A—H49C | 0.9900 |
C14—H14B | 0.9800 | C49A—H49D | 0.9900 |
C14—H14C | 0.9800 | C49A—C50Aii | 1.575 (7) |
C15—C16 | 1.447 (5) | C50A—H50A | 1.0000 |
C15—C20 | 1.406 (4) | C50A—C51 | 1.484 (6) |
C16—C17 | 1.427 (4) | C51—C53 | 1.3900 |
C17—C18 | 1.388 (4) | C51—C52 | 1.3900 |
C17—C21 | 1.528 (5) | C53—H53 | 0.9500 |
C18—H18 | 0.9500 | C53—C55 | 1.3900 |
C18—C19 | 1.418 (5) | C55—H55 | 0.9500 |
C19—C20 | 1.380 (5) | C55—N4 | 1.3900 |
C19—C25 | 1.544 (5) | N4—C54 | 1.3900 |
C20—H20 | 0.9500 | C54—H54 | 0.9500 |
C21—C22 | 1.540 (5) | C54—C52 | 1.3900 |
C21—C23 | 1.521 (5) | C52—H52 | 0.9500 |
C21—C24 | 1.543 (5) | C26—H26A | 0.9800 |
C22—H22A | 0.9800 | C26—H26B | 0.9800 |
C22—H22B | 0.9800 | C26—H26C | 0.9800 |
C22—H22C | 0.9800 | C27—H27A | 0.9800 |
C23—H23A | 0.9800 | C27—H27B | 0.9800 |
C23—H23B | 0.9800 | C27—H27C | 0.9800 |
C23—H23C | 0.9800 | C28—H28A | 0.9800 |
C24—H24A | 0.9800 | C28—H28B | 0.9800 |
C24—H24B | 0.9800 | C28—H28C | 0.9800 |
C24—H24C | 0.9800 | C0AA—H0AA | 0.9800 |
C25—C26 | 1.630 (7) | C0AA—H0AB | 0.9800 |
C25—C27 | 1.482 (5) | C0AA—H0AC | 0.9800 |
C25—C28 | 1.497 (7) | C1AA—H1AA | 0.9800 |
C25—C0AA | 1.488 (7) | C1AA—H1AB | 0.9800 |
C25—C1AA | 1.470 (7) | C1AA—H1AC | 0.9800 |
C25—C2AA | 1.612 (8) | C2AA—H2AA | 0.9800 |
C29—H29 | 0.9500 | C2AA—H2AB | 0.9800 |
C29—C32 | 1.390 (4) | C2AA—H2AC | 0.9800 |
C30—H30 | 0.9500 | O7—H7 | 0.8400 |
C30—C31 | 1.386 (4) | O7—C01L | 1.444 (8) |
C31—H31 | 0.9500 | C01L—H01A | 0.9900 |
C31—C33 | 1.386 (5) | C01L—H01B | 0.9900 |
C32—H32 | 0.9500 | C01L—C01U | 1.451 (10) |
C32—C33 | 1.393 (4) | C01U—H01C | 0.9800 |
C33—C34 | 1.529 (4) | C01U—H01D | 0.9800 |
C33—C34A | 1.529 (4) | C01U—H01E | 0.9800 |
C34—H34 | 1.0000 | | |
| | | |
O1—Co1—O2 | 88.39 (11) | C33—C34—C36 | 110.5 (3) |
O1—Co1—O3 | 88.19 (11) | C33—C34—C37i | 109.2 (3) |
O1—Co1—O4 | 91.63 (12) | C36—C34—H34 | 109.5 |
O1—Co1—N1 | 88.40 (11) | C36—C34—C37i | 108.8 (3) |
O1—Co1—N3 | 178.52 (11) | C37i—C34—H34 | 109.5 |
O2—Co1—O3 | 175.44 (11) | C34—C36—H36A | 109.2 |
O2—Co1—O4 | 90.99 (11) | C34—C36—H36B | 109.2 |
O2—Co1—N1 | 90.96 (11) | C34—C36—C37 | 112.2 (3) |
O2—Co1—N3 | 92.99 (11) | H36A—C36—H36B | 107.9 |
O3—Co1—O4 | 86.09 (10) | C37—C36—H36A | 109.2 |
O3—Co1—N1 | 91.96 (11) | C37—C36—H36B | 109.2 |
O3—Co1—N3 | 90.46 (11) | O6—C37—C36 | 103.9 (5) |
O4—Co1—N1 | 178.05 (11) | O6—C37—C38 | 115.9 (6) |
O4—Co1—N3 | 88.89 (12) | C38—C37—C36 | 111.4 (3) |
N1—Co1—N3 | 91.04 (12) | C37—O6—H6A | 109.5 |
C2—O1—Co1 | 109.5 (2) | C33—C34A—C36A | 110.5 (3) |
C1—O2—Co1 | 108.0 (2) | O6A—C34A—C33 | 109.9 (4) |
C16—O3—Co1 | 110.9 (2) | O6A—C34A—C36A | 108.5 (4) |
C15—O4—Co1 | 110.1 (2) | C34A—O6A—H6AA | 109.5 |
C29—N1—Co1 | 121.3 (2) | C34A—C36A—H36C | 109.2 |
C29—N1—C30 | 117.7 (3) | C34A—C36A—H36D | 109.2 |
C30—N1—Co1 | 120.9 (2) | C34A—C36A—C37A | 112.2 (3) |
C41—N2—C40 | 117.8 (3) | H36C—C36A—H36D | 107.9 |
C43—N3—Co1 | 122.9 (3) | C37A—C36A—H36C | 109.2 |
C43—N3—C45 | 117.5 (3) | C37A—C36A—H36D | 109.2 |
C45—N3—Co1 | 119.3 (3) | C34Ai—C37A—H37A | 108.4 |
O2—C1—C2 | 117.2 (3) | C36A—C37A—H37A | 108.4 |
O2—C1—C6 | 122.2 (3) | C38—C37A—C34Ai | 111.0 (3) |
C6—C1—C2 | 120.6 (3) | C38—C37A—C36A | 111.4 (3) |
O1—C2—C1 | 115.3 (3) | C38—C37A—H37A | 108.4 |
O1—C2—C3 | 124.1 (3) | C39—C38—C37 | 122.4 (3) |
C3—C2—C1 | 120.5 (3) | C39—C38—C37A | 122.4 (3) |
C2—C3—C11 | 120.1 (3) | C42—C38—C37 | 121.2 (3) |
C4—C3—C2 | 116.8 (3) | C42—C38—C37A | 121.2 (3) |
C4—C3—C11 | 123.1 (3) | C42—C38—C39 | 116.5 (3) |
C3—C4—H4 | 118.1 | C38—C39—H39 | 120.3 |
C3—C4—C5 | 123.7 (3) | C40—C39—C38 | 119.4 (3) |
C5—C4—H4 | 118.1 | C40—C39—H39 | 120.3 |
C4—C5—C7 | 120.3 (3) | N2—C40—C39 | 123.3 (4) |
C6—C5—C4 | 117.8 (3) | N2—C40—H40 | 118.4 |
C6—C5—C7 | 121.8 (3) | C39—C40—H40 | 118.4 |
C1—C6—H6 | 119.7 | N2—C41—H41 | 118.7 |
C5—C6—C1 | 120.5 (3) | N2—C41—C42 | 122.7 (4) |
C5—C6—H6 | 119.7 | C42—C41—H41 | 118.7 |
C5—C7—C8 | 112.5 (3) | C38—C42—H42 | 119.8 |
C5—C7—C9 | 108.9 (4) | C41—C42—C38 | 120.3 (4) |
C8—C7—C9 | 105.4 (4) | C41—C42—H42 | 119.8 |
C10—C7—C5 | 110.9 (4) | N3—C43—H43 | 111 (4) |
C10—C7—C8 | 110.4 (4) | N3—C43—C44 | 122.1 (4) |
C10—C7—C9 | 108.6 (5) | C44—C43—H43 | 126 (4) |
C7—C8—H8A | 109.5 | C43—C44—H44 | 114 (3) |
C7—C8—H8B | 109.5 | C43—C44—C47 | 119.5 (4) |
C7—C8—H8C | 109.5 | C47—C44—H44 | 125 (3) |
H8A—C8—H8B | 109.5 | N3—C45—H45 | 118 (3) |
H8A—C8—H8C | 109.5 | N3—C45—C46 | 123.6 (4) |
H8B—C8—H8C | 109.5 | C46—C45—H45 | 118 (3) |
C7—C9—H9A | 109.5 | C45—C46—H46 | 120.4 |
C7—C9—H9B | 109.5 | C45—C46—C47 | 119.1 (4) |
C7—C9—H9C | 109.5 | C47—C46—H46 | 120.4 |
H9A—C9—H9B | 109.5 | C44—C47—C48 | 129.5 (5) |
H9A—C9—H9C | 109.5 | C44—C47—C48A | 129.5 (5) |
H9B—C9—H9C | 109.5 | C46—C47—C44 | 118.0 (4) |
C7—C10—H10A | 109.5 | C46—C47—C48 | 112.4 (5) |
C7—C10—H10B | 109.5 | C46—C47—C48A | 112.4 (5) |
C7—C10—H10C | 109.5 | C47—C48—H48 | 108.7 |
H10A—C10—H10B | 109.5 | C49—C48—C47 | 111.3 (4) |
H10A—C10—H10C | 109.5 | C49—C48—H48 | 108.7 |
H10B—C10—H10C | 109.5 | C49—C48—C50 | 112.2 (4) |
C3—C11—C12 | 110.5 (3) | C50—C48—C47 | 107.1 (5) |
C3—C11—C14 | 111.9 (3) | C50—C48—H48 | 108.7 |
C13—C11—C3 | 110.2 (3) | C48—C49—H49A | 109.2 |
C13—C11—C12 | 107.6 (3) | C48—C49—H49B | 109.2 |
C13—C11—C14 | 108.7 (3) | C48—C49—C50ii | 111.9 (4) |
C14—C11—C12 | 107.8 (3) | H49A—C49—H49B | 107.9 |
C11—C12—H12A | 109.5 | C50ii—C49—H49A | 109.2 |
C11—C12—H12B | 109.5 | C50ii—C49—H49B | 109.2 |
C11—C12—H12C | 109.5 | O5—C50—C48 | 102.5 (8) |
H12A—C12—H12B | 109.5 | O5—C50—C51 | 101.5 (9) |
H12A—C12—H12C | 109.5 | C51—C50—C48 | 115.9 (4) |
H12B—C12—H12C | 109.5 | C50—O5—H5 | 109.5 |
C11—C13—H13A | 109.5 | O5A—C48A—C47 | 115.8 (8) |
C11—C13—H13B | 109.5 | O5A—C48A—C49A | 120.3 (9) |
C11—C13—H13C | 109.5 | O5A—C48A—C50A | 86.9 (9) |
H13A—C13—H13B | 109.5 | C49A—C48A—C47 | 111.3 (4) |
H13A—C13—H13C | 109.5 | C49A—C48A—C50A | 112.2 (4) |
H13B—C13—H13C | 109.5 | C50A—C48A—C47 | 107.1 (5) |
C11—C14—H14A | 109.5 | C48A—O5A—H5A | 109.5 |
C11—C14—H14B | 109.5 | C48A—C49A—H49C | 109.2 |
C11—C14—H14C | 109.5 | C48A—C49A—H49D | 109.2 |
H14A—C14—H14B | 109.5 | H49C—C49A—H49D | 107.9 |
H14A—C14—H14C | 109.5 | C50Aii—C49A—H49C | 109.2 |
H14B—C14—H14C | 109.5 | C50Aii—C49A—H49D | 109.2 |
O4—C15—C16 | 117.0 (3) | C48A—C50A—H50A | 107.2 |
O4—C15—C20 | 123.2 (3) | C49Aii—C50A—H50A | 107.2 |
C20—C15—C16 | 119.8 (3) | C51—C50A—C48A | 115.9 (4) |
O3—C16—C15 | 115.8 (3) | C51—C50A—C49Aii | 109.5 (4) |
O3—C16—C17 | 123.7 (3) | C51—C50A—H50A | 107.2 |
C17—C16—C15 | 120.4 (3) | C53—C51—C50 | 117.7 (3) |
C16—C17—C21 | 120.6 (3) | C53—C51—C50A | 117.7 (3) |
C18—C17—C16 | 116.5 (3) | C53—C51—C52 | 120.0 |
C18—C17—C21 | 122.8 (3) | C52—C51—C50 | 122.3 (3) |
C17—C18—H18 | 118.1 | C52—C51—C50A | 122.3 (3) |
C17—C18—C19 | 123.8 (3) | C51—C53—H53 | 120.0 |
C19—C18—H18 | 118.1 | C51—C53—C55 | 120.0 |
C18—C19—C25 | 120.0 (3) | C55—C53—H53 | 120.0 |
C20—C19—C18 | 119.3 (3) | C53—C55—H55 | 120.0 |
C20—C19—C25 | 120.7 (3) | N4—C55—C53 | 120.0 |
C15—C20—H20 | 120.0 | N4—C55—H55 | 120.0 |
C19—C20—C15 | 120.1 (3) | C55—N4—C54 | 120.0 |
C19—C20—H20 | 120.0 | N4—C54—H54 | 120.0 |
C17—C21—C22 | 109.5 (3) | C52—C54—N4 | 120.0 |
C17—C21—C24 | 111.7 (3) | C52—C54—H54 | 120.0 |
C22—C21—C24 | 107.6 (3) | C51—C52—H52 | 120.0 |
C23—C21—C17 | 110.5 (3) | C54—C52—C51 | 120.0 |
C23—C21—C22 | 109.7 (3) | C54—C52—H52 | 120.0 |
C23—C21—C24 | 107.8 (3) | C25—C26—H26A | 109.5 |
C21—C22—H22A | 109.5 | C25—C26—H26B | 109.5 |
C21—C22—H22B | 109.5 | C25—C26—H26C | 109.5 |
C21—C22—H22C | 109.5 | H26A—C26—H26B | 109.5 |
H22A—C22—H22B | 109.5 | H26A—C26—H26C | 109.5 |
H22A—C22—H22C | 109.5 | H26B—C26—H26C | 109.5 |
H22B—C22—H22C | 109.5 | C25—C27—H27A | 109.5 |
C21—C23—H23A | 109.5 | C25—C27—H27B | 109.5 |
C21—C23—H23B | 109.5 | C25—C27—H27C | 109.5 |
C21—C23—H23C | 109.5 | H27A—C27—H27B | 109.5 |
H23A—C23—H23B | 109.5 | H27A—C27—H27C | 109.5 |
H23A—C23—H23C | 109.5 | H27B—C27—H27C | 109.5 |
H23B—C23—H23C | 109.5 | C25—C28—H28A | 109.5 |
C21—C24—H24A | 109.5 | C25—C28—H28B | 109.5 |
C21—C24—H24B | 109.5 | C25—C28—H28C | 109.5 |
C21—C24—H24C | 109.5 | H28A—C28—H28B | 109.5 |
H24A—C24—H24B | 109.5 | H28A—C28—H28C | 109.5 |
H24A—C24—H24C | 109.5 | H28B—C28—H28C | 109.5 |
H24B—C24—H24C | 109.5 | C25—C0AA—H0AA | 109.5 |
C19—C25—C26 | 105.0 (4) | C25—C0AA—H0AB | 109.5 |
C19—C25—C2AA | 100.8 (6) | C25—C0AA—H0AC | 109.5 |
C27—C25—C19 | 115.6 (4) | H0AA—C0AA—H0AB | 109.5 |
C27—C25—C26 | 104.9 (5) | H0AA—C0AA—H0AC | 109.5 |
C27—C25—C28 | 115.1 (5) | H0AB—C0AA—H0AC | 109.5 |
C28—C25—C19 | 110.9 (4) | C25—C1AA—H1AA | 109.5 |
C28—C25—C26 | 103.9 (5) | C25—C1AA—H1AB | 109.5 |
C0AA—C25—C19 | 110.7 (5) | C25—C1AA—H1AC | 109.5 |
C0AA—C25—C2AA | 105.5 (6) | H1AA—C1AA—H1AB | 109.5 |
C1AA—C25—C19 | 115.1 (5) | H1AA—C1AA—H1AC | 109.5 |
C1AA—C25—C0AA | 116.8 (6) | H1AB—C1AA—H1AC | 109.5 |
C1AA—C25—C2AA | 106.0 (6) | C25—C2AA—H2AA | 109.5 |
N1—C29—H29 | 118.9 | C25—C2AA—H2AB | 109.5 |
N1—C29—C32 | 122.1 (3) | C25—C2AA—H2AC | 109.5 |
C32—C29—H29 | 118.9 | H2AA—C2AA—H2AB | 109.5 |
N1—C30—H30 | 118.6 | H2AA—C2AA—H2AC | 109.5 |
N1—C30—C31 | 122.9 (3) | H2AB—C2AA—H2AC | 109.5 |
C31—C30—H30 | 118.6 | C01L—O7—H7 | 109.5 |
C30—C31—H31 | 120.0 | O7—C01L—H01A | 110.0 |
C30—C31—C33 | 120.0 (3) | O7—C01L—H01B | 110.0 |
C33—C31—H31 | 120.0 | O7—C01L—C01U | 108.6 (7) |
C29—C32—H32 | 119.8 | H01A—C01L—H01B | 108.4 |
C29—C32—C33 | 120.3 (3) | C01U—C01L—H01A | 110.0 |
C33—C32—H32 | 119.8 | C01U—C01L—H01B | 110.0 |
C31—C33—C32 | 117.0 (3) | C01L—C01U—H01C | 109.5 |
C31—C33—C34 | 122.1 (3) | C01L—C01U—H01D | 109.5 |
C31—C33—C34A | 122.1 (3) | C01L—C01U—H01E | 109.5 |
C32—C33—C34 | 120.8 (3) | H01C—C01U—H01D | 109.5 |
C32—C33—C34A | 120.8 (3) | H01C—C01U—H01E | 109.5 |
C33—C34—H34 | 109.5 | H01D—C01U—H01E | 109.5 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+2, −y+1, −z+2. |
catena-Poly[[[(3,5-di-
tert-butylbenzene-1,2-diolato)(1,5-di-
tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)cobalt(III)]-µ-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]–ethanol–water (1/1/5)] (2_275k)
top
Crystal data top
[Co(C14H20O2)2(C26H24N4O)]·C2H6O·5H2O | Z = 2 |
Mr = 1044.17 | F(000) = 1118 |
Triclinic, P1 | Dx = 1.240 Mg m−3 |
a = 10.066 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 16.124 (3) Å | Cell parameters from 15234 reflections |
c = 18.205 (4) Å | θ = 1.2–32.3° |
α = 75.36 (3)° | µ = 0.37 mm−1 |
β = 83.11 (3)° | T = 275 K |
γ = 78.68 (3)° | Plate, clear blue |
V = 2795.5 (11) Å3 | 0.1 × 0.04 × 0.02 mm |
Data collection top
ADSC Quantum 210r diffractometer | 17440 independent reflections |
Radiation source: MX1 Beamline Australian Synchrotron | 11405 reflections with I > 2σ(I) |
Silicon Double Crystal monochromator | Rint = 0.073 |
Phi Scan scans | θmax = 32.3°, θmin = 1.2° |
Absorption correction: multi-scan SADABS-2012/1 (Bruker,2012) | h = −14→14 |
Tmin = 0.963, Tmax = 0.993 | k = −23→24 |
110832 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.087 | w = 1/[σ2(Fo2) + (0.1329P)2 + 3.0137P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.269 | (Δ/σ)max = 0.001 |
S = 1.05 | Δρmax = 1.58 e Å−3 |
17440 reflections | Δρmin = −0.82 e Å−3 |
673 parameters | Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
80 restraints | Extinction coefficient: 0.065 (4) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Crystals were small and weakly scattering, hence data collection was carried
out at the Australian Synchrotron. Some of the crystals were disordered, the
crystals showed minor disorder, however the Rint value was still relatively
high. During the refinement it was found the structure was disordered: the
alcohol group of the tpch ligand is disordered over four positions on the
cyclohexane ring and so refinement was carried out with these atoms restrained
to ideal geometry. One of the tert-butyl groups also displays disorder and so
refinement was carried out with these groups disordered over two components,
both being restrained to ideal geometry. The maximum residual electron
density peaks, 1.65 eA-3, were close one of the pydidyl groups of the tpch
ligand indicating that this group was somewhat disordered. Attempts to model
this disorder were not successful. The disorder required a number of distance
and angle constraints and restraints to ensure the disordered components were
maintained at a chemical reasonable geometry. The displacement parameters of
each of the atoms of each component were constrained to be equal. The increase
in data collection temperature, from 100K to 275K, has resulted in increased
thermal motion of several of the atoms, requiring an increase in the number of
distance and angle restraints to maintain chemically reasonable geometry.
The crystal showed a solvent void containing disordered/diffuse solvent
consistent with 5 molecules of water per formula unit (containing one cobalt
atom). There were six reflections OMITted due to anomalous background. The
high final R and wR values are a consequence of the disorder of the crystals. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.38430 (4) | 0.57620 (2) | 0.77484 (2) | 0.03447 (14) | |
O1 | 0.2376 (2) | 0.57599 (14) | 0.72176 (14) | 0.0451 (5) | |
O2 | 0.2654 (2) | 0.64775 (15) | 0.82888 (13) | 0.0442 (5) | |
O3 | 0.4902 (2) | 0.49778 (13) | 0.72006 (12) | 0.0407 (5) | |
O4 | 0.3493 (3) | 0.47383 (15) | 0.84897 (14) | 0.0486 (5) | |
N1 | 0.4260 (2) | 0.67736 (15) | 0.69664 (14) | 0.0346 (5) | |
N2 | 0.9798 (3) | 1.1221 (2) | 0.5260 (2) | 0.0617 (9) | |
N3 | 0.5420 (3) | 0.57488 (17) | 0.82894 (15) | 0.0413 (6) | |
C1 | 0.1492 (3) | 0.67370 (19) | 0.79565 (18) | 0.0410 (6) | |
C2 | 0.1332 (3) | 0.63593 (19) | 0.73674 (18) | 0.0398 (6) | |
C3 | 0.0163 (4) | 0.6613 (2) | 0.6976 (2) | 0.0461 (7) | |
C4 | −0.0826 (4) | 0.7245 (2) | 0.7206 (2) | 0.0509 (8) | |
H4 | −0.161446 | 0.742740 | 0.694812 | 0.061* | |
C5 | −0.0714 (4) | 0.7622 (2) | 0.7796 (2) | 0.0515 (8) | |
C6 | 0.0475 (4) | 0.7362 (2) | 0.8164 (2) | 0.0459 (7) | |
H6 | 0.058967 | 0.761000 | 0.855616 | 0.055* | |
C7 | −0.1853 (4) | 0.8309 (3) | 0.8019 (3) | 0.0646 (11) | |
C8 | −0.1593 (8) | 0.8574 (5) | 0.8720 (4) | 0.115 (3) | |
H8A | −0.171855 | 0.811437 | 0.916189 | 0.172* | |
H8B | −0.221737 | 0.909288 | 0.876919 | 0.172* | |
H8C | −0.067900 | 0.868132 | 0.867610 | 0.172* | |
C9 | −0.3143 (6) | 0.7897 (5) | 0.8285 (5) | 0.111 (2) | |
H9A | −0.349424 | 0.779051 | 0.785634 | 0.166* | |
H9B | −0.381632 | 0.828653 | 0.851203 | 0.166* | |
H9C | −0.292018 | 0.735670 | 0.865328 | 0.166* | |
C10 | −0.2108 (11) | 0.9055 (5) | 0.7381 (4) | 0.162 (4) | |
H10A | −0.126242 | 0.923102 | 0.715962 | 0.243* | |
H10B | −0.268589 | 0.952697 | 0.755536 | 0.243* | |
H10C | −0.254484 | 0.890199 | 0.700543 | 0.243* | |
C11 | 0.0026 (4) | 0.6229 (3) | 0.6318 (2) | 0.0558 (9) | |
C12 | 0.0162 (5) | 0.5234 (3) | 0.6578 (3) | 0.0668 (11) | |
H12A | 0.019968 | 0.499429 | 0.614219 | 0.100* | |
H12B | −0.060747 | 0.508622 | 0.691748 | 0.100* | |
H12C | 0.097903 | 0.499877 | 0.683644 | 0.100* | |
C13 | 0.1152 (5) | 0.6427 (3) | 0.5699 (2) | 0.0641 (10) | |
H13A | 0.111018 | 0.704545 | 0.553392 | 0.096* | |
H13B | 0.103959 | 0.619892 | 0.527634 | 0.096* | |
H13C | 0.201687 | 0.616199 | 0.589700 | 0.096* | |
C14 | −0.1337 (5) | 0.6588 (4) | 0.5977 (3) | 0.0769 (13) | |
H14A | −0.144623 | 0.721096 | 0.581719 | 0.115* | |
H14B | −0.205515 | 0.642789 | 0.635225 | 0.115* | |
H14C | −0.136953 | 0.635277 | 0.554635 | 0.115* | |
C15 | 0.4085 (3) | 0.40470 (19) | 0.82710 (19) | 0.0427 (7) | |
C16 | 0.4849 (3) | 0.41768 (18) | 0.75460 (18) | 0.0394 (6) | |
C17 | 0.5485 (4) | 0.3455 (2) | 0.7260 (2) | 0.0449 (7) | |
C18 | 0.5378 (4) | 0.2651 (2) | 0.7710 (2) | 0.0550 (9) | |
H18 | 0.579982 | 0.216690 | 0.752842 | 0.066* | |
C19 | 0.4670 (5) | 0.2509 (2) | 0.8430 (2) | 0.0613 (10) | |
C20 | 0.4025 (4) | 0.3208 (2) | 0.8703 (2) | 0.0570 (9) | |
H20 | 0.354543 | 0.312358 | 0.917724 | 0.068* | |
C21 | 0.6254 (4) | 0.3591 (2) | 0.6477 (2) | 0.0534 (8) | |
C22 | 0.7434 (5) | 0.4067 (3) | 0.6467 (3) | 0.0759 (13) | |
H22A | 0.708085 | 0.465337 | 0.650641 | 0.114* | |
H22B | 0.799110 | 0.407434 | 0.600005 | 0.114* | |
H22C | 0.796887 | 0.377131 | 0.688963 | 0.114* | |
C23 | 0.5311 (6) | 0.4106 (3) | 0.5882 (3) | 0.0777 (14) | |
H23A | 0.453954 | 0.382598 | 0.591767 | 0.117* | |
H23B | 0.577882 | 0.413882 | 0.538615 | 0.117* | |
H23C | 0.501187 | 0.468217 | 0.595976 | 0.117* | |
C24 | 0.6851 (6) | 0.2724 (3) | 0.6273 (3) | 0.0813 (15) | |
H24A | 0.739628 | 0.236037 | 0.666952 | 0.122* | |
H24B | 0.740362 | 0.282654 | 0.580220 | 0.122* | |
H24C | 0.612676 | 0.243971 | 0.621862 | 0.122* | |
C25 | 0.4620 (6) | 0.1582 (3) | 0.8908 (3) | 0.0877 (17) | |
C29 | 0.4490 (3) | 0.67498 (18) | 0.62404 (18) | 0.0403 (6) | |
H29 | 0.447908 | 0.623200 | 0.610567 | 0.048* | |
C30 | 0.4260 (4) | 0.7527 (2) | 0.71424 (19) | 0.0468 (7) | |
H30 | 0.408877 | 0.755832 | 0.764907 | 0.056* | |
C31 | 0.4504 (4) | 0.8261 (2) | 0.6604 (2) | 0.0525 (9) | |
H31 | 0.450906 | 0.877160 | 0.675175 | 0.063* | |
C32 | 0.4744 (3) | 0.74672 (19) | 0.56736 (18) | 0.0411 (6) | |
H32 | 0.492021 | 0.742030 | 0.517109 | 0.049* | |
C33 | 0.4739 (3) | 0.82449 (18) | 0.58492 (18) | 0.0393 (6) | |
C34 | 0.4956 (3) | 0.90524 (18) | 0.52424 (18) | 0.0409 (6) | 0.694 (3) |
H34 | 0.517510 | 0.889526 | 0.475037 | 0.049* | 0.694 (3) |
C36 | 0.6106 (3) | 0.94376 (19) | 0.5406 (2) | 0.0450 (7) | 0.5 |
H36A | 0.692876 | 0.900462 | 0.543341 | 0.054* | 0.5 |
H36B | 0.590260 | 0.957910 | 0.589912 | 0.054* | 0.5 |
C37 | 0.6364 (3) | 1.02593 (19) | 0.48051 (18) | 0.0417 (7) | 0.194 (3) |
O6 | 0.6543 (15) | 1.0000 (8) | 0.4087 (4) | 0.060 (4) | 0.194 (3) |
H6A | 0.687845 | 0.948298 | 0.415771 | 0.090* | 0.194 (3) |
C34A | 0.4956 (3) | 0.90524 (18) | 0.52424 (18) | 0.0409 (6) | 0.306 (3) |
O6A | 0.5310 (7) | 0.8808 (4) | 0.4495 (4) | 0.0358 (14) | 0.306 (3) |
H6AA | 0.610659 | 0.856767 | 0.447265 | 0.054* | 0.306 (3) |
C36A | 0.6106 (3) | 0.94376 (19) | 0.5406 (2) | 0.0450 (7) | 0.5 |
H36C | 0.692876 | 0.900462 | 0.543341 | 0.054* | 0.5 |
H36D | 0.590260 | 0.957910 | 0.589912 | 0.054* | 0.5 |
C37A | 0.6364 (3) | 1.02593 (19) | 0.48051 (18) | 0.0417 (7) | 0.806 (3) |
H37A | 0.657463 | 1.010693 | 0.431084 | 0.050* | 0.806 (3) |
C38 | 0.7549 (3) | 1.06079 (19) | 0.4971 (2) | 0.0447 (7) | |
C39 | 0.7698 (4) | 1.0700 (2) | 0.5689 (2) | 0.0505 (8) | |
H39 | 0.704193 | 1.056835 | 0.608535 | 0.061* | |
C40 | 0.8829 (4) | 1.0989 (2) | 0.5808 (3) | 0.0599 (10) | |
H40 | 0.893228 | 1.102750 | 0.629841 | 0.072* | |
C41 | 0.9621 (4) | 1.1142 (3) | 0.4584 (3) | 0.0622 (10) | |
H41 | 1.027452 | 1.129662 | 0.419261 | 0.075* | |
C42 | 0.8539 (4) | 1.0847 (2) | 0.4413 (2) | 0.0555 (9) | |
H42 | 0.847381 | 1.080755 | 0.391754 | 0.067* | |
C43 | 0.5323 (4) | 0.5741 (2) | 0.9020 (2) | 0.0526 (8) | |
H43 | 0.446704 | 0.583820 | 0.927141 | 0.11 (2)* | |
C44 | 0.6458 (5) | 0.5594 (3) | 0.9419 (3) | 0.0658 (11) | |
H44 | 0.636233 | 0.557840 | 0.993678 | 0.058 (12)* | |
C45 | 0.6646 (4) | 0.5656 (3) | 0.7935 (2) | 0.0539 (8) | |
H45 | 0.671839 | 0.567990 | 0.741653 | 0.052 (11)* | |
C46 | 0.7805 (4) | 0.5528 (3) | 0.8291 (3) | 0.0662 (11) | |
H46 | 0.864390 | 0.547969 | 0.801407 | 0.079* | |
C47 | 0.7742 (5) | 0.5469 (3) | 0.9051 (3) | 0.0707 (13) | |
C48 | 0.9063 (6) | 0.5261 (4) | 0.9418 (4) | 0.105 (2) | 0.814 (3) |
H48 | 0.973276 | 0.541602 | 0.899284 | 0.126* | 0.814 (3) |
C49 | 0.9132 (4) | 0.5850 (2) | 0.9915 (2) | 0.0527 (8) | 0.5 |
H49A | 0.840143 | 0.579806 | 1.031390 | 0.063* | 0.5 |
H49B | 0.899564 | 0.644636 | 0.961593 | 0.063* | 0.5 |
C50 | 0.9507 (5) | 0.4348 (3) | 0.9719 (3) | 0.0747 (12) | 0.314 (3) |
O5 | 0.8313 (8) | 0.4194 (11) | 1.0230 (6) | 0.110 (5) | 0.314 (3) |
H5 | 0.817140 | 0.453213 | 1.051108 | 0.165* | 0.314 (3) |
C48A | 0.9063 (6) | 0.5261 (4) | 0.9418 (4) | 0.105 (2) | 0.186 (3) |
O5A | 1.0309 (14) | 0.5351 (10) | 0.8939 (8) | 0.113 (7) | 0.186 (3) |
H5A | 1.094168 | 0.500239 | 0.914531 | 0.170* | 0.186 (3) |
C49A | 0.9132 (4) | 0.5850 (2) | 0.9915 (2) | 0.0527 (8) | 0.5 |
H49C | 0.840143 | 0.579806 | 1.031390 | 0.063* | 0.5 |
H49D | 0.899564 | 0.644636 | 0.961593 | 0.063* | 0.5 |
C50A | 0.9507 (5) | 0.4348 (3) | 0.9719 (3) | 0.0747 (12) | 0.686 (3) |
H50A | 0.883964 | 0.418224 | 1.014308 | 0.090* | 0.686 (3) |
C51 | 0.9517 (4) | 0.3758 (2) | 0.9235 (2) | 0.0663 (11) | |
C53 | 0.8535 (4) | 0.3226 (3) | 0.9432 (3) | 0.158 (3) | |
H53 | 0.793340 | 0.325565 | 0.985752 | 0.189* | |
C55 | 0.8453 (5) | 0.2651 (3) | 0.8991 (4) | 0.229 (6) | |
H55 | 0.779612 | 0.229521 | 0.912268 | 0.275* | |
N4 | 0.9352 (7) | 0.2607 (3) | 0.8355 (4) | 0.187 (4) | |
C54 | 1.0334 (5) | 0.3139 (4) | 0.8159 (3) | 0.161 (4) | |
H54 | 1.093590 | 0.310960 | 0.773270 | 0.193* | |
C52 | 1.0416 (4) | 0.3714 (3) | 0.8599 (2) | 0.111 (2) | |
H52 | 1.107320 | 0.407005 | 0.846752 | 0.133* | |
C26 | 0.5198 (15) | 0.1507 (6) | 0.9691 (6) | 0.116 (5) | 0.5 |
H26A | 0.609612 | 0.164791 | 0.960200 | 0.174* | 0.5 |
H26B | 0.523384 | 0.092297 | 0.999458 | 0.174* | 0.5 |
H26C | 0.461873 | 0.190372 | 0.995449 | 0.174* | 0.5 |
C27 | 0.5445 (16) | 0.0894 (7) | 0.8548 (8) | 0.117 (6) | 0.5 |
H27A | 0.525657 | 0.101788 | 0.802284 | 0.175* | 0.5 |
H27B | 0.521550 | 0.033819 | 0.880797 | 0.175* | 0.5 |
H27C | 0.639256 | 0.088416 | 0.858095 | 0.175* | 0.5 |
C28 | 0.3146 (9) | 0.1463 (8) | 0.9090 (9) | 0.099 (4) | 0.5 |
H28A | 0.267507 | 0.188080 | 0.936716 | 0.148* | 0.5 |
H28B | 0.310717 | 0.088605 | 0.939243 | 0.148* | 0.5 |
H28C | 0.272408 | 0.154858 | 0.862439 | 0.148* | 0.5 |
C26A | 0.6019 (16) | 0.1061 (9) | 0.8952 (10) | 0.118 (6) | 0.5 |
H26D | 0.650393 | 0.117599 | 0.846034 | 0.177* | 0.5 |
H26E | 0.596675 | 0.045250 | 0.911292 | 0.177* | 0.5 |
H26F | 0.648812 | 0.121810 | 0.931235 | 0.177* | 0.5 |
C27A | 0.367 (2) | 0.1509 (8) | 0.9528 (10) | 0.119 (5) | 0.5 |
H27D | 0.395905 | 0.172436 | 0.991737 | 0.178* | 0.5 |
H27E | 0.358247 | 0.090913 | 0.972376 | 0.178* | 0.5 |
H27F | 0.280707 | 0.184313 | 0.937260 | 0.178* | 0.5 |
C28A | 0.397 (3) | 0.1159 (10) | 0.8296 (12) | 0.168 (9) | 0.5 |
H28D | 0.314121 | 0.153167 | 0.812297 | 0.251* | 0.5 |
H28E | 0.377671 | 0.059135 | 0.855139 | 0.251* | 0.5 |
H28F | 0.461037 | 0.111400 | 0.786851 | 0.251* | 0.5 |
O7 | 1.1924 (5) | 1.1587 (4) | 0.5866 (4) | 0.1249 (19) | |
H7 | 1.140159 | 1.153823 | 0.557283 | 0.187* | |
C56 | 1.1364 (10) | 1.2347 (7) | 0.6180 (6) | 0.151 (3) | |
H56A | 1.077959 | 1.218125 | 0.663714 | 0.182* | |
H56B | 1.083085 | 1.279004 | 0.581224 | 0.182* | |
C57 | 1.2517 (12) | 1.2687 (12) | 0.6361 (10) | 0.269 (10) | |
H57A | 1.322311 | 1.267999 | 0.595711 | 0.403* | |
H57B | 1.286131 | 1.232921 | 0.682845 | 0.403* | |
H57C | 1.221486 | 1.327331 | 0.641453 | 0.403* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0359 (2) | 0.02480 (19) | 0.0373 (2) | −0.00252 (13) | −0.00335 (14) | 0.00074 (13) |
O1 | 0.0483 (12) | 0.0378 (11) | 0.0495 (13) | −0.0074 (9) | −0.0025 (10) | −0.0114 (9) |
O2 | 0.0467 (12) | 0.0411 (11) | 0.0424 (11) | −0.0019 (9) | −0.0067 (9) | −0.0081 (9) |
O3 | 0.0475 (12) | 0.0291 (9) | 0.0400 (11) | −0.0037 (8) | 0.0010 (9) | −0.0026 (8) |
O4 | 0.0517 (13) | 0.0381 (11) | 0.0504 (13) | −0.0073 (10) | 0.0094 (10) | −0.0070 (10) |
N1 | 0.0384 (12) | 0.0266 (10) | 0.0350 (11) | −0.0060 (9) | −0.0070 (9) | 0.0019 (8) |
N2 | 0.0536 (18) | 0.0453 (16) | 0.088 (3) | −0.0088 (14) | −0.0097 (17) | −0.0156 (16) |
N3 | 0.0402 (13) | 0.0357 (12) | 0.0411 (13) | −0.0007 (10) | −0.0068 (10) | 0.0006 (10) |
C1 | 0.0442 (16) | 0.0335 (13) | 0.0411 (15) | −0.0058 (12) | −0.0019 (12) | −0.0021 (11) |
C2 | 0.0424 (15) | 0.0332 (13) | 0.0420 (15) | −0.0092 (11) | 0.0009 (12) | −0.0055 (11) |
C3 | 0.0460 (17) | 0.0424 (16) | 0.0500 (18) | −0.0130 (13) | −0.0018 (14) | −0.0080 (13) |
C4 | 0.0421 (17) | 0.0504 (18) | 0.059 (2) | −0.0059 (14) | −0.0082 (15) | −0.0099 (16) |
C5 | 0.0436 (17) | 0.0421 (16) | 0.066 (2) | −0.0040 (13) | −0.0045 (16) | −0.0109 (15) |
C6 | 0.0484 (18) | 0.0368 (15) | 0.0494 (17) | −0.0053 (13) | −0.0030 (14) | −0.0064 (13) |
C7 | 0.054 (2) | 0.058 (2) | 0.078 (3) | 0.0120 (17) | −0.012 (2) | −0.023 (2) |
C8 | 0.130 (6) | 0.105 (5) | 0.094 (4) | 0.051 (4) | −0.013 (4) | −0.048 (4) |
C9 | 0.063 (3) | 0.120 (5) | 0.149 (6) | 0.008 (3) | 0.005 (4) | −0.054 (5) |
C10 | 0.235 (9) | 0.089 (4) | 0.095 (4) | 0.084 (5) | 0.023 (5) | 0.000 (4) |
C11 | 0.056 (2) | 0.060 (2) | 0.055 (2) | −0.0173 (17) | −0.0041 (16) | −0.0138 (17) |
C12 | 0.081 (3) | 0.062 (2) | 0.069 (3) | −0.030 (2) | −0.005 (2) | −0.024 (2) |
C13 | 0.066 (2) | 0.075 (3) | 0.050 (2) | −0.015 (2) | 0.0005 (18) | −0.0118 (19) |
C14 | 0.064 (3) | 0.099 (4) | 0.077 (3) | −0.012 (2) | −0.022 (2) | −0.031 (3) |
C15 | 0.0407 (15) | 0.0326 (13) | 0.0475 (16) | −0.0029 (11) | −0.0004 (13) | 0.0000 (12) |
C16 | 0.0407 (15) | 0.0283 (12) | 0.0436 (15) | −0.0029 (11) | −0.0017 (12) | −0.0016 (11) |
C17 | 0.0493 (17) | 0.0334 (14) | 0.0483 (17) | −0.0036 (12) | −0.0015 (14) | −0.0063 (12) |
C18 | 0.065 (2) | 0.0305 (14) | 0.062 (2) | −0.0038 (14) | 0.0045 (17) | −0.0047 (14) |
C19 | 0.075 (3) | 0.0298 (14) | 0.065 (2) | −0.0043 (15) | 0.0103 (19) | 0.0049 (14) |
C20 | 0.065 (2) | 0.0399 (16) | 0.055 (2) | −0.0126 (15) | 0.0142 (17) | 0.0027 (15) |
C21 | 0.070 (2) | 0.0399 (16) | 0.0489 (18) | −0.0100 (15) | 0.0050 (16) | −0.0126 (14) |
C22 | 0.070 (3) | 0.080 (3) | 0.084 (3) | −0.029 (2) | 0.029 (2) | −0.035 (3) |
C23 | 0.114 (4) | 0.068 (3) | 0.048 (2) | −0.010 (3) | −0.009 (2) | −0.012 (2) |
C24 | 0.109 (4) | 0.050 (2) | 0.078 (3) | −0.006 (2) | 0.025 (3) | −0.022 (2) |
C25 | 0.111 (4) | 0.0349 (18) | 0.094 (4) | −0.013 (2) | 0.025 (3) | 0.012 (2) |
C29 | 0.0504 (17) | 0.0268 (12) | 0.0418 (15) | −0.0083 (11) | −0.0039 (13) | −0.0030 (11) |
C30 | 0.068 (2) | 0.0319 (14) | 0.0409 (16) | −0.0131 (14) | −0.0058 (14) | −0.0046 (12) |
C31 | 0.083 (3) | 0.0294 (14) | 0.0451 (17) | −0.0183 (15) | −0.0020 (17) | −0.0043 (12) |
C32 | 0.0503 (17) | 0.0303 (13) | 0.0392 (15) | −0.0076 (12) | −0.0056 (12) | −0.0006 (11) |
C33 | 0.0437 (15) | 0.0270 (12) | 0.0429 (15) | −0.0051 (11) | −0.0085 (12) | 0.0013 (11) |
C34 | 0.0462 (16) | 0.0268 (12) | 0.0433 (15) | −0.0053 (11) | −0.0039 (12) | 0.0031 (11) |
C36 | 0.0453 (16) | 0.0291 (13) | 0.0536 (18) | −0.0059 (11) | −0.0070 (14) | 0.0045 (12) |
C37 | 0.0444 (16) | 0.0293 (13) | 0.0452 (16) | −0.0063 (11) | −0.0039 (13) | 0.0030 (11) |
O6 | 0.057 (8) | 0.046 (7) | 0.064 (8) | −0.007 (6) | −0.004 (6) | 0.008 (6) |
C34A | 0.0462 (16) | 0.0268 (12) | 0.0433 (15) | −0.0053 (11) | −0.0039 (12) | 0.0031 (11) |
O6A | 0.037 (3) | 0.029 (3) | 0.039 (3) | −0.004 (2) | −0.006 (3) | −0.004 (2) |
C36A | 0.0453 (16) | 0.0291 (13) | 0.0536 (18) | −0.0059 (11) | −0.0070 (14) | 0.0045 (12) |
C37A | 0.0444 (16) | 0.0293 (13) | 0.0452 (16) | −0.0063 (11) | −0.0039 (13) | 0.0030 (11) |
C38 | 0.0447 (16) | 0.0287 (13) | 0.0549 (18) | −0.0026 (11) | −0.0068 (14) | −0.0008 (12) |
C39 | 0.056 (2) | 0.0359 (15) | 0.0549 (19) | −0.0020 (14) | −0.0091 (16) | −0.0045 (14) |
C40 | 0.060 (2) | 0.0405 (17) | 0.080 (3) | −0.0010 (15) | −0.016 (2) | −0.0159 (17) |
C41 | 0.051 (2) | 0.052 (2) | 0.079 (3) | −0.0129 (16) | 0.0044 (19) | −0.0067 (19) |
C42 | 0.057 (2) | 0.0452 (18) | 0.060 (2) | −0.0131 (15) | 0.0007 (17) | −0.0044 (16) |
C43 | 0.059 (2) | 0.0485 (18) | 0.0447 (17) | −0.0029 (15) | −0.0048 (15) | −0.0043 (14) |
C44 | 0.080 (3) | 0.059 (2) | 0.055 (2) | 0.004 (2) | −0.023 (2) | −0.0107 (18) |
C45 | 0.0425 (18) | 0.060 (2) | 0.053 (2) | −0.0016 (15) | −0.0059 (15) | −0.0078 (16) |
C46 | 0.0413 (19) | 0.077 (3) | 0.080 (3) | 0.0063 (18) | −0.0132 (18) | −0.026 (2) |
C47 | 0.063 (2) | 0.065 (2) | 0.088 (3) | 0.0204 (19) | −0.039 (2) | −0.033 (2) |
C48 | 0.093 (4) | 0.089 (4) | 0.147 (6) | 0.038 (3) | −0.078 (4) | −0.064 (4) |
C49 | 0.057 (2) | 0.0473 (18) | 0.0472 (18) | 0.0041 (15) | −0.0131 (15) | −0.0044 (14) |
C50 | 0.0749 (15) | 0.0737 (15) | 0.0748 (15) | −0.0100 (9) | −0.0100 (9) | −0.0166 (9) |
O5 | 0.063 (6) | 0.171 (14) | 0.053 (6) | −0.010 (8) | −0.007 (5) | 0.046 (7) |
C48A | 0.093 (4) | 0.089 (4) | 0.147 (6) | 0.038 (3) | −0.078 (4) | −0.064 (4) |
O5A | 0.068 (9) | 0.140 (12) | 0.110 (11) | −0.054 (9) | 0.005 (8) | 0.031 (9) |
C49A | 0.057 (2) | 0.0473 (18) | 0.0472 (18) | 0.0041 (15) | −0.0131 (15) | −0.0044 (14) |
C50A | 0.0749 (15) | 0.0737 (15) | 0.0748 (15) | −0.0100 (9) | −0.0100 (9) | −0.0166 (9) |
C51 | 0.059 (2) | 0.055 (2) | 0.083 (3) | −0.0034 (18) | −0.028 (2) | −0.007 (2) |
C53 | 0.154 (5) | 0.139 (5) | 0.190 (5) | −0.044 (4) | 0.003 (4) | −0.051 (4) |
C55 | 0.232 (8) | 0.233 (8) | 0.240 (8) | −0.064 (5) | −0.018 (5) | −0.072 (5) |
N4 | 0.206 (6) | 0.174 (5) | 0.206 (5) | −0.042 (4) | −0.025 (4) | −0.076 (4) |
C54 | 0.160 (5) | 0.168 (5) | 0.147 (5) | 0.002 (4) | −0.018 (4) | −0.044 (4) |
C52 | 0.087 (4) | 0.148 (6) | 0.099 (4) | 0.029 (4) | −0.035 (4) | −0.056 (4) |
C26 | 0.170 (14) | 0.057 (6) | 0.100 (9) | −0.022 (7) | −0.051 (9) | 0.042 (6) |
C27 | 0.164 (14) | 0.039 (5) | 0.118 (11) | 0.000 (7) | 0.024 (10) | 0.007 (6) |
C28 | 0.109 (7) | 0.066 (6) | 0.118 (8) | −0.045 (5) | 0.001 (6) | 0.003 (6) |
C26A | 0.120 (11) | 0.057 (7) | 0.131 (13) | 0.014 (7) | 0.000 (9) | 0.034 (8) |
C27A | 0.152 (12) | 0.057 (6) | 0.117 (10) | −0.028 (7) | 0.037 (9) | 0.020 (7) |
C28A | 0.26 (3) | 0.075 (9) | 0.168 (17) | −0.090 (13) | −0.039 (17) | 0.028 (10) |
O7 | 0.077 (3) | 0.147 (4) | 0.180 (5) | 0.000 (3) | −0.023 (3) | −0.100 (4) |
C56 | 0.189 (10) | 0.156 (8) | 0.128 (7) | −0.051 (7) | −0.036 (7) | −0.041 (6) |
C57 | 0.177 (12) | 0.37 (2) | 0.36 (2) | −0.135 (14) | 0.025 (13) | −0.23 (2) |
Geometric parameters (Å, º) top
Co1—O1 | 1.860 (2) | C34—C36 | 1.508 (5) |
Co1—O2 | 1.865 (2) | C34—C37i | 1.550 (4) |
Co1—O3 | 1.893 (2) | C36—H36A | 0.9700 |
Co1—O4 | 1.912 (2) | C36—H36B | 0.9700 |
Co1—N1 | 1.953 (2) | C36—C37 | 1.534 (4) |
Co1—N3 | 1.960 (3) | C37—O6 | 1.4504 (11) |
O1—C2 | 1.333 (4) | C37—C38 | 1.505 (5) |
O2—C1 | 1.326 (4) | O6—H6A | 0.8200 |
O3—C16 | 1.294 (3) | C34A—O6A | 1.495 (7) |
O4—C15 | 1.289 (4) | C34A—C36A | 1.508 (5) |
N1—C29 | 1.323 (4) | O6A—H6AA | 0.8200 |
N1—C30 | 1.333 (4) | C36A—H36C | 0.9700 |
N2—C40 | 1.344 (6) | C36A—H36D | 0.9700 |
N2—C41 | 1.306 (6) | C36A—C37A | 1.534 (4) |
N3—C43 | 1.319 (5) | C37A—H37A | 0.9800 |
N3—C45 | 1.322 (5) | C37A—C38 | 1.505 (5) |
C1—C2 | 1.399 (5) | C38—C39 | 1.381 (5) |
C1—C6 | 1.379 (5) | C38—C42 | 1.372 (5) |
C2—C3 | 1.387 (5) | C39—H39 | 0.9300 |
C3—C4 | 1.387 (5) | C39—C40 | 1.370 (6) |
C3—C11 | 1.512 (5) | C40—H40 | 0.9300 |
C4—H4 | 0.9300 | C41—H41 | 0.9300 |
C4—C5 | 1.386 (5) | C41—C42 | 1.368 (6) |
C5—C6 | 1.382 (5) | C42—H42 | 0.9300 |
C5—C7 | 1.524 (5) | C43—H43 | 0.9300 |
C6—H6 | 0.9300 | C43—C44 | 1.377 (6) |
C7—C8 | 1.510 (8) | C44—H44 | 0.9300 |
C7—C9 | 1.546 (8) | C44—C47 | 1.386 (7) |
C7—C10 | 1.451 (8) | C45—H45 | 0.9300 |
C8—H8A | 0.9600 | C45—C46 | 1.358 (5) |
C8—H8B | 0.9600 | C46—H46 | 0.9300 |
C8—H8C | 0.9600 | C46—C47 | 1.357 (7) |
C9—H9A | 0.9600 | C47—C48 | 1.501 (6) |
C9—H9B | 0.9600 | C47—C48A | 1.501 (6) |
C9—H9C | 0.9600 | C48—H48 | 0.9800 |
C10—H10A | 0.9600 | C48—C49 | 1.483 (6) |
C10—H10B | 0.9600 | C48—C50 | 1.435 (8) |
C10—H10C | 0.9600 | C49—H49A | 0.9700 |
C11—C12 | 1.537 (6) | C49—H49B | 0.9700 |
C11—C13 | 1.520 (6) | C49—C50ii | 1.537 (6) |
C11—C14 | 1.521 (6) | C50—O5 | 1.4507 (11) |
C12—H12A | 0.9600 | C50—C51 | 1.448 (6) |
C12—H12B | 0.9600 | O5—H5 | 0.8200 |
C12—H12C | 0.9600 | C48A—O5A | 1.4500 (11) |
C13—H13A | 0.9600 | C48A—C49A | 1.483 (6) |
C13—H13B | 0.9600 | C48A—C50A | 1.435 (8) |
C13—H13C | 0.9600 | O5A—H5A | 0.8200 |
C14—H14A | 0.9600 | C49A—H49C | 0.9700 |
C14—H14B | 0.9600 | C49A—H49D | 0.9700 |
C14—H14C | 0.9600 | C49A—C50Aii | 1.537 (6) |
C15—C16 | 1.434 (4) | C50A—H50A | 0.9800 |
C15—C20 | 1.391 (4) | C50A—C51 | 1.448 (6) |
C16—C17 | 1.404 (4) | C51—C53 | 1.3900 |
C17—C18 | 1.364 (5) | C51—C52 | 1.3900 |
C17—C21 | 1.524 (5) | C53—H53 | 0.9300 |
C18—H18 | 0.9300 | C53—C55 | 1.3900 |
C18—C19 | 1.403 (5) | C55—H55 | 0.9300 |
C19—C20 | 1.361 (5) | C55—N4 | 1.3900 |
C19—C25 | 1.535 (5) | N4—C54 | 1.3900 |
C20—H20 | 0.9300 | C54—H54 | 0.9300 |
C21—C22 | 1.532 (6) | C54—C52 | 1.3900 |
C21—C23 | 1.499 (6) | C52—H52 | 0.9300 |
C21—C24 | 1.527 (5) | C26—H26A | 0.9600 |
C22—H22A | 0.9600 | C26—H26B | 0.9600 |
C22—H22B | 0.9600 | C26—H26C | 0.9600 |
C22—H22C | 0.9600 | C27—H27A | 0.9600 |
C23—H23A | 0.9600 | C27—H27B | 0.9600 |
C23—H23B | 0.9600 | C27—H27C | 0.9600 |
C23—H23C | 0.9600 | C28—H28A | 0.9600 |
C24—H24A | 0.9600 | C28—H28B | 0.9600 |
C24—H24B | 0.9600 | C28—H28C | 0.9600 |
C24—H24C | 0.9600 | C26A—H26D | 0.9600 |
C25—C26 | 1.571 (7) | C26A—H26E | 0.9600 |
C25—C27 | 1.492 (6) | C26A—H26F | 0.9600 |
C25—C28 | 1.519 (7) | C27A—H27D | 0.9600 |
C25—C26A | 1.492 (15) | C27A—H27E | 0.9600 |
C25—C27A | 1.386 (14) | C27A—H27F | 0.9600 |
C25—C28A | 1.70 (2) | C28A—H28D | 0.9600 |
C29—H29 | 0.9300 | C28A—H28E | 0.9600 |
C29—C32 | 1.385 (4) | C28A—H28F | 0.9600 |
C30—H30 | 0.9300 | O7—H7 | 0.8200 |
C30—C31 | 1.375 (4) | O7—C56 | 1.467 (10) |
C31—H31 | 0.9300 | C56—H56A | 0.9700 |
C31—C33 | 1.371 (5) | C56—H56B | 0.9700 |
C32—H32 | 0.9300 | C56—C57 | 1.4796 (11) |
C32—C33 | 1.369 (4) | C57—H57A | 0.9600 |
C33—C34 | 1.513 (4) | C57—H57B | 0.9600 |
C33—C34A | 1.513 (4) | C57—H57C | 0.9600 |
C34—H34 | 0.9800 | | |
| | | |
O1—Co1—O2 | 87.35 (10) | C33—C34—C37i | 109.8 (3) |
O1—Co1—O3 | 88.02 (10) | C36—C34—C33 | 111.4 (3) |
O1—Co1—O4 | 91.56 (11) | C36—C34—H34 | 108.8 |
O1—Co1—N1 | 88.70 (10) | C36—C34—C37i | 109.3 (3) |
O1—Co1—N3 | 178.52 (11) | C37i—C34—H34 | 108.8 |
O2—Co1—O3 | 174.26 (10) | C34—C36—H36A | 108.9 |
O2—Co1—O4 | 91.60 (10) | C34—C36—H36B | 108.9 |
O2—Co1—N1 | 91.02 (11) | C34—C36—C37 | 113.3 (3) |
O2—Co1—N3 | 94.11 (11) | H36A—C36—H36B | 107.7 |
O3—Co1—O4 | 85.13 (10) | C37—C36—H36A | 108.9 |
O3—Co1—N1 | 92.27 (10) | C37—C36—H36B | 108.9 |
O3—Co1—N3 | 90.54 (11) | O6—C37—C36 | 104.6 (6) |
O4—Co1—N1 | 177.37 (10) | O6—C37—C38 | 114.1 (6) |
O4—Co1—N3 | 88.62 (11) | C38—C37—C36 | 111.9 (3) |
N1—Co1—N3 | 91.06 (11) | C37—O6—H6A | 109.5 |
C2—O1—Co1 | 109.8 (2) | O6A—C34A—C33 | 108.6 (3) |
C1—O2—Co1 | 108.9 (2) | O6A—C34A—C36A | 108.2 (4) |
C16—O3—Co1 | 111.6 (2) | C36A—C34A—C33 | 111.4 (3) |
C15—O4—Co1 | 110.8 (2) | C34A—O6A—H6AA | 109.5 |
C29—N1—Co1 | 121.5 (2) | C34A—C36A—H36C | 108.9 |
C29—N1—C30 | 117.5 (3) | C34A—C36A—H36D | 108.9 |
C30—N1—Co1 | 120.9 (2) | C34A—C36A—C37A | 113.3 (3) |
C41—N2—C40 | 115.7 (4) | H36C—C36A—H36D | 107.7 |
C43—N3—Co1 | 122.4 (3) | C37A—C36A—H36C | 108.9 |
C43—N3—C45 | 118.1 (3) | C37A—C36A—H36D | 108.9 |
C45—N3—Co1 | 119.2 (2) | C34Ai—C37A—H37A | 108.1 |
O2—C1—C2 | 117.3 (3) | C36A—C37A—H37A | 108.1 |
O2—C1—C6 | 122.5 (3) | C38—C37A—C34Ai | 111.7 (3) |
C6—C1—C2 | 120.2 (3) | C38—C37A—C36A | 111.9 (3) |
O1—C2—C1 | 115.1 (3) | C38—C37A—H37A | 108.1 |
O1—C2—C3 | 124.0 (3) | C39—C38—C37 | 121.9 (3) |
C3—C2—C1 | 120.9 (3) | C39—C38—C37A | 121.9 (3) |
C2—C3—C11 | 120.5 (3) | C42—C38—C37 | 121.3 (3) |
C4—C3—C2 | 116.6 (3) | C42—C38—C37A | 121.3 (3) |
C4—C3—C11 | 122.9 (3) | C42—C38—C39 | 116.8 (3) |
C3—C4—H4 | 117.9 | C38—C39—H39 | 120.6 |
C5—C4—C3 | 124.1 (3) | C40—C39—C38 | 118.9 (4) |
C5—C4—H4 | 117.9 | C40—C39—H39 | 120.6 |
C4—C5—C7 | 121.0 (3) | N2—C40—C39 | 124.2 (4) |
C6—C5—C4 | 117.5 (3) | N2—C40—H40 | 117.9 |
C6—C5—C7 | 121.5 (4) | C39—C40—H40 | 117.9 |
C1—C6—C5 | 120.6 (3) | N2—C41—H41 | 117.8 |
C1—C6—H6 | 119.7 | N2—C41—C42 | 124.4 (4) |
C5—C6—H6 | 119.7 | C42—C41—H41 | 117.8 |
C5—C7—C9 | 108.7 (4) | C38—C42—H42 | 120.0 |
C8—C7—C5 | 112.7 (4) | C41—C42—C38 | 120.0 (4) |
C8—C7—C9 | 102.1 (5) | C41—C42—H42 | 120.0 |
C10—C7—C5 | 110.5 (4) | N3—C43—H43 | 119.2 |
C10—C7—C8 | 111.7 (6) | N3—C43—C44 | 121.6 (4) |
C10—C7—C9 | 110.7 (6) | C44—C43—H43 | 119.2 |
C7—C8—H8A | 109.5 | C43—C44—H44 | 120.0 |
C7—C8—H8B | 109.5 | C43—C44—C47 | 120.1 (4) |
C7—C8—H8C | 109.5 | C47—C44—H44 | 120.0 |
H8A—C8—H8B | 109.5 | N3—C45—H45 | 118.4 |
H8A—C8—H8C | 109.5 | N3—C45—C46 | 123.3 (4) |
H8B—C8—H8C | 109.5 | C46—C45—H45 | 118.4 |
C7—C9—H9A | 109.5 | C45—C46—H46 | 120.0 |
C7—C9—H9B | 109.5 | C47—C46—C45 | 120.1 (4) |
C7—C9—H9C | 109.5 | C47—C46—H46 | 120.0 |
H9A—C9—H9B | 109.5 | C44—C47—C48 | 125.9 (5) |
H9A—C9—H9C | 109.5 | C44—C47—C48A | 125.9 (5) |
H9B—C9—H9C | 109.5 | C46—C47—C44 | 116.8 (4) |
C7—C10—H10A | 109.5 | C46—C47—C48 | 117.3 (5) |
C7—C10—H10B | 109.5 | C46—C47—C48A | 117.3 (5) |
C7—C10—H10C | 109.5 | C47—C48—H48 | 103.9 |
H10A—C10—H10B | 109.5 | C49—C48—C47 | 112.6 (4) |
H10A—C10—H10C | 109.5 | C49—C48—H48 | 103.9 |
H10B—C10—H10C | 109.5 | C50—C48—C47 | 113.8 (5) |
C3—C11—C12 | 110.7 (3) | C50—C48—H48 | 103.9 |
C3—C11—C13 | 109.9 (3) | C50—C48—C49 | 116.9 (5) |
C3—C11—C14 | 111.8 (4) | C48—C49—H49A | 109.0 |
C13—C11—C12 | 107.4 (4) | C48—C49—H49B | 109.0 |
C13—C11—C14 | 108.7 (4) | C48—C49—C50ii | 112.9 (4) |
C14—C11—C12 | 108.2 (4) | H49A—C49—H49B | 107.8 |
C11—C12—H12A | 109.5 | C50ii—C49—H49A | 109.0 |
C11—C12—H12B | 109.5 | C50ii—C49—H49B | 109.0 |
C11—C12—H12C | 109.5 | C48—C50—O5 | 97.0 (8) |
H12A—C12—H12B | 109.5 | C48—C50—C51 | 118.3 (4) |
H12A—C12—H12C | 109.5 | C51—C50—O5 | 101.3 (8) |
H12B—C12—H12C | 109.5 | C50—O5—H5 | 109.5 |
C11—C13—H13A | 109.5 | O5A—C48A—C47 | 118.9 (9) |
C11—C13—H13B | 109.5 | O5A—C48A—C49A | 100.1 (5) |
C11—C13—H13C | 109.5 | C49A—C48A—C47 | 112.6 (4) |
H13A—C13—H13B | 109.5 | C50A—C48A—C47 | 113.8 (5) |
H13A—C13—H13C | 109.5 | C50A—C48A—O5A | 92.8 (8) |
H13B—C13—H13C | 109.5 | C50A—C48A—C49A | 116.9 (5) |
C11—C14—H14A | 109.5 | C48A—O5A—H5A | 109.5 |
C11—C14—H14B | 109.5 | C48A—C49A—H49C | 109.0 |
C11—C14—H14C | 109.5 | C48A—C49A—H49D | 109.0 |
H14A—C14—H14B | 109.5 | H49C—C49A—H49D | 107.8 |
H14A—C14—H14C | 109.5 | C50Aii—C49A—H49C | 109.0 |
H14B—C14—H14C | 109.5 | C50Aii—C49A—H49D | 109.0 |
O4—C15—C16 | 116.5 (3) | C48A—C50A—H50A | 104.8 |
O4—C15—C20 | 123.5 (3) | C48A—C50A—C51 | 118.3 (4) |
C20—C15—C16 | 120.0 (3) | C49Aii—C50A—H50A | 104.8 |
O3—C16—C15 | 115.8 (3) | C51—C50A—C49Aii | 109.9 (4) |
O3—C16—C17 | 124.5 (3) | C51—C50A—H50A | 104.8 |
C17—C16—C15 | 119.7 (3) | C53—C51—C50 | 116.0 (3) |
C16—C17—C21 | 119.9 (3) | C53—C51—C50A | 116.0 (3) |
C18—C17—C16 | 117.2 (3) | C53—C51—C52 | 120.0 |
C18—C17—C21 | 122.9 (3) | C52—C51—C50 | 124.0 (3) |
C17—C18—H18 | 118.0 | C52—C51—C50A | 124.0 (3) |
C17—C18—C19 | 124.0 (3) | C51—C53—H53 | 120.0 |
C19—C18—H18 | 118.0 | C55—C53—C51 | 120.0 |
C18—C19—C25 | 120.8 (4) | C55—C53—H53 | 120.0 |
C20—C19—C18 | 119.0 (3) | C53—C55—H55 | 120.0 |
C20—C19—C25 | 120.2 (4) | C53—C55—N4 | 120.0 |
C15—C20—H20 | 120.0 | N4—C55—H55 | 120.0 |
C19—C20—C15 | 120.0 (3) | C54—N4—C55 | 120.0 |
C19—C20—H20 | 120.0 | N4—C54—H54 | 120.0 |
C17—C21—C22 | 110.0 (3) | N4—C54—C52 | 120.0 |
C17—C21—C24 | 111.4 (3) | C52—C54—H54 | 120.0 |
C23—C21—C17 | 110.0 (4) | C51—C52—H52 | 120.0 |
C23—C21—C22 | 110.0 (4) | C54—C52—C51 | 120.0 |
C23—C21—C24 | 107.8 (4) | C54—C52—H52 | 120.0 |
C24—C21—C22 | 107.6 (4) | C25—C26—H26A | 109.5 |
C21—C22—H22A | 109.5 | C25—C26—H26B | 109.5 |
C21—C22—H22B | 109.5 | C25—C26—H26C | 109.5 |
C21—C22—H22C | 109.5 | H26A—C26—H26B | 109.5 |
H22A—C22—H22B | 109.5 | H26A—C26—H26C | 109.5 |
H22A—C22—H22C | 109.5 | H26B—C26—H26C | 109.5 |
H22B—C22—H22C | 109.5 | C25—C27—H27A | 109.5 |
C21—C23—H23A | 109.5 | C25—C27—H27B | 109.5 |
C21—C23—H23B | 109.5 | C25—C27—H27C | 109.5 |
C21—C23—H23C | 109.5 | H27A—C27—H27B | 109.5 |
H23A—C23—H23B | 109.5 | H27A—C27—H27C | 109.5 |
H23A—C23—H23C | 109.5 | H27B—C27—H27C | 109.5 |
H23B—C23—H23C | 109.5 | C25—C28—H28A | 109.5 |
C21—C24—H24A | 109.5 | C25—C28—H28B | 109.5 |
C21—C24—H24B | 109.5 | C25—C28—H28C | 109.5 |
C21—C24—H24C | 109.5 | H28A—C28—H28B | 109.5 |
H24A—C24—H24B | 109.5 | H28A—C28—H28C | 109.5 |
H24A—C24—H24C | 109.5 | H28B—C28—H28C | 109.5 |
H24B—C24—H24C | 109.5 | C25—C26A—H26D | 109.5 |
C19—C25—C26 | 107.1 (5) | C25—C26A—H26E | 109.5 |
C19—C25—C28A | 100.9 (6) | C25—C26A—H26F | 109.5 |
C27—C25—C19 | 113.3 (6) | H26D—C26A—H26E | 109.5 |
C27—C25—C26 | 108.6 (6) | H26D—C26A—H26F | 109.5 |
C27—C25—C28 | 112.2 (6) | H26E—C26A—H26F | 109.5 |
C28—C25—C19 | 109.1 (6) | C25—C27A—H27D | 109.5 |
C28—C25—C26 | 106.2 (6) | C25—C27A—H27E | 109.5 |
C26A—C25—C19 | 110.0 (6) | C25—C27A—H27F | 109.5 |
C26A—C25—C28A | 101.3 (12) | H27D—C27A—H27E | 109.5 |
C27A—C25—C19 | 115.9 (6) | H27D—C27A—H27F | 109.5 |
C27A—C25—C26A | 122.0 (10) | H27E—C27A—H27F | 109.5 |
C27A—C25—C28A | 102.9 (12) | C25—C28A—H28D | 109.5 |
N1—C29—H29 | 118.8 | C25—C28A—H28E | 109.5 |
N1—C29—C32 | 122.5 (3) | C25—C28A—H28F | 109.5 |
C32—C29—H29 | 118.8 | H28D—C28A—H28E | 109.5 |
N1—C30—H30 | 118.7 | H28D—C28A—H28F | 109.5 |
N1—C30—C31 | 122.5 (3) | H28E—C28A—H28F | 109.5 |
C31—C30—H30 | 118.7 | C56—O7—H7 | 109.5 |
C30—C31—H31 | 119.8 | O7—C56—H56A | 110.1 |
C33—C31—C30 | 120.4 (3) | O7—C56—H56B | 110.1 |
C33—C31—H31 | 119.8 | O7—C56—C57 | 107.8 (9) |
C29—C32—H32 | 119.8 | H56A—C56—H56B | 108.5 |
C33—C32—C29 | 120.4 (3) | C57—C56—H56A | 110.1 |
C33—C32—H32 | 119.8 | C57—C56—H56B | 110.1 |
C31—C33—C34 | 121.4 (3) | C56—C57—H57A | 109.5 |
C31—C33—C34A | 121.4 (3) | C56—C57—H57B | 109.5 |
C32—C33—C31 | 116.6 (3) | C56—C57—H57C | 109.5 |
C32—C33—C34 | 121.9 (3) | H57A—C57—H57B | 109.5 |
C32—C33—C34A | 121.9 (3) | H57A—C57—H57C | 109.5 |
C33—C34—H34 | 108.8 | H57B—C57—H57C | 109.5 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+2, −y+1, −z+2. |
catena-Poly[[[(3,5-di-
tert-butylbenzene-1,2-diolato)(1,5-di-
tert-butyl-4-oxocyclohexa-2,5-dien-1-yl-3-olato)cobalt(III)]-µ-1-hydroxy-1,2,4,5-tetrakis(pyridin-4-yl)cyclohexane]–ethanol–water (1/1/5)] (2_315k)
top
Crystal data top
[Co(C14H20O2)2(C26H24N4O)]·C2H6O·3H2O | Z = 2 |
Mr = 1008.13 | F(000) = 1078 |
Triclinic, P1 | Dx = 1.152 Mg m−3 |
a = 10.168 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 16.321 (3) Å | Cell parameters from 107805 reflections |
c = 18.515 (4) Å | θ = 1.9–33.5° |
α = 75.33 (3)° | µ = 0.35 mm−1 |
β = 82.77 (3)° | T = 315 K |
γ = 78.77 (3)° | Plate, clear blue |
V = 2906.0 (11) Å3 | 0.1 × 0.04 × 0.02 mm |
Data collection top
ADSC Quantum 210r diffractometer | 17669 independent reflections |
Radiation source: MX1 Beamline Australian Synchrotron | 10358 reflections with I > 2σ(I) |
Silicon Double Crystal monochromator | Rint = 0.101 |
Phi Scan scans | θmax = 32.0°, θmin = 1.1° |
Absorption correction: multi-scan SADABS-2012/1 (Bruker,2012) | h = −14→14 |
Tmin = 0.963, Tmax = 0.993 | k = −23→24 |
194018 measured reflections | l = −26→26 |
Refinement top
Refinement on F2 | Hydrogen site location: mixed |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.100 | w = 1/[σ2(Fo2) + (0.1729P)2 + 2.2991P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.330 | (Δ/σ)max = 0.001 |
S = 1.03 | Δρmax = 1.16 e Å−3 |
17669 reflections | Δρmin = −0.52 e Å−3 |
679 parameters | Extinction correction: SHELXL2018 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
139 restraints | Extinction coefficient: 0.089 (7) |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Crystals were small and weakly scattering, hence data collection was carried
out at the Australian Synchrotron. Some of the crystals were disordered, the
crystals showed minor disorder, however the Rint value was still relatively
high. During the refinement it was found the structure was disordered: the
alcohol group of the tpch ligand is disordered over four positions on the
cyclohexane ring and so refinement was carried out with these atoms restrained
to ideal geometry. One of the tert-butyl groups also displays disorder and so
refinement was carried out with these groups disordered over two components,
both being restrained to ideal geometry. The maximum residual electron
density peaks, 1.16 eA-3, were close one of the pydidyl groups of the tpch
ligand indicating that this group was somewhat disordered. Attempts to model
this disorder were not successful. The disorder required a number of distance
and angle constraints and restraints to ensure the disordered components were
maintained at a chemical reasonable geometry. The displacement parameters of
each of the atoms of each component were constrained to be equal. The increase
in data collection temperature, from 100K to 275K to 315K, has resulted in
increased thermal motion of several of the atoms, requiring an increase in
the number of distance and angle restraints to maintain chemically reasonable
geometry.
The crystal showed a solvent void containing disordered/diffuse solvent
consistent with 3 molecules of water per formula unit (containing one cobalt
atom) - a loss of 2 molecules of water from the 100K and 275K structures.
There were seven reflections OMITted due to anomalous background. The high
final R and wR values are a consequence of the disorder of the crystals. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.38294 (5) | 0.57691 (3) | 0.77597 (3) | 0.0513 (2) | |
O1 | 0.2330 (3) | 0.57719 (18) | 0.72202 (17) | 0.0706 (7) | |
O2 | 0.2588 (3) | 0.64832 (18) | 0.82957 (16) | 0.0686 (7) | |
O3 | 0.4873 (3) | 0.49703 (16) | 0.72065 (15) | 0.0617 (6) | |
O4 | 0.3491 (3) | 0.47223 (19) | 0.85082 (17) | 0.0702 (7) | |
N1 | 0.4254 (3) | 0.67946 (17) | 0.69595 (16) | 0.0509 (6) | |
N2 | 0.9773 (4) | 1.1223 (3) | 0.5264 (3) | 0.0877 (12) | |
N3 | 0.5420 (3) | 0.5759 (2) | 0.83076 (19) | 0.0618 (8) | |
C1 | 0.1450 (4) | 0.6746 (2) | 0.7960 (2) | 0.0609 (9) | |
C2 | 0.1298 (4) | 0.6364 (2) | 0.7365 (2) | 0.0598 (9) | |
C3 | 0.0128 (4) | 0.6624 (3) | 0.6973 (2) | 0.0655 (10) | |
C4 | −0.0848 (5) | 0.7252 (3) | 0.7198 (3) | 0.0736 (11) | |
H4 | −0.162170 | 0.743634 | 0.694125 | 0.088* | |
C5 | −0.0743 (5) | 0.7629 (3) | 0.7792 (3) | 0.0742 (11) | |
C6 | 0.0432 (4) | 0.7369 (3) | 0.8154 (3) | 0.0673 (10) | |
H6 | 0.054010 | 0.761825 | 0.853781 | 0.081* | |
C7 | −0.1880 (6) | 0.8304 (3) | 0.8016 (3) | 0.0892 (15) | |
C8 | −0.1657 (10) | 0.8570 (6) | 0.8725 (5) | 0.151 (4) | |
H8A | −0.160249 | 0.807750 | 0.914046 | 0.226* | |
H8B | −0.239536 | 0.900085 | 0.882861 | 0.226* | |
H8C | −0.083488 | 0.879742 | 0.864747 | 0.226* | |
C9 | −0.3158 (8) | 0.7922 (6) | 0.8277 (6) | 0.155 (4) | |
H9A | −0.367470 | 0.800502 | 0.785611 | 0.233* | |
H9B | −0.368051 | 0.820146 | 0.864273 | 0.233* | |
H9C | −0.292600 | 0.731825 | 0.849491 | 0.233* | |
C10 | −0.2162 (14) | 0.9059 (5) | 0.7384 (4) | 0.209 (6) | |
H10A | −0.135338 | 0.929290 | 0.720468 | 0.313* | |
H10B | −0.283721 | 0.948663 | 0.754935 | 0.313* | |
H10C | −0.247854 | 0.888681 | 0.698689 | 0.313* | |
C11 | −0.0004 (5) | 0.6243 (3) | 0.6309 (3) | 0.0795 (12) | |
C12 | 0.0127 (7) | 0.5248 (4) | 0.6575 (4) | 0.0977 (17) | |
H12A | 0.017920 | 0.500618 | 0.614836 | 0.147* | |
H12B | −0.064469 | 0.510580 | 0.690498 | 0.147* | |
H12C | 0.092620 | 0.501981 | 0.683500 | 0.147* | |
C13 | 0.1139 (5) | 0.6431 (4) | 0.5701 (3) | 0.0867 (14) | |
H13A | 0.116685 | 0.703598 | 0.557279 | 0.130* | |
H13B | 0.098814 | 0.625684 | 0.526510 | 0.130* | |
H13C | 0.197985 | 0.611903 | 0.588515 | 0.130* | |
C14 | −0.1359 (6) | 0.6605 (5) | 0.5976 (4) | 0.108 (2) | |
H14A | −0.147110 | 0.722108 | 0.583309 | 0.163* | |
H14B | −0.207109 | 0.643445 | 0.634281 | 0.163* | |
H14C | −0.138630 | 0.638751 | 0.554361 | 0.163* | |
C15 | 0.4084 (4) | 0.4043 (2) | 0.8280 (2) | 0.0613 (9) | |
C16 | 0.4824 (4) | 0.4174 (2) | 0.7553 (2) | 0.0568 (8) | |
C17 | 0.5466 (4) | 0.3459 (2) | 0.7263 (2) | 0.0648 (9) | |
C18 | 0.5367 (5) | 0.2657 (3) | 0.7709 (3) | 0.0784 (12) | |
H18 | 0.578037 | 0.218023 | 0.752716 | 0.094* | |
C19 | 0.4671 (6) | 0.2513 (3) | 0.8430 (3) | 0.0830 (14) | |
C20 | 0.4044 (5) | 0.3199 (3) | 0.8707 (3) | 0.0791 (13) | |
H20 | 0.358614 | 0.311062 | 0.918015 | 0.095* | |
C21 | 0.6238 (5) | 0.3593 (3) | 0.6475 (3) | 0.0757 (12) | |
C22 | 0.7387 (7) | 0.4087 (5) | 0.6451 (4) | 0.116 (2) | |
H22A | 0.702357 | 0.463906 | 0.655132 | 0.174* | |
H22B | 0.786506 | 0.416187 | 0.596372 | 0.174* | |
H22C | 0.799121 | 0.376838 | 0.682221 | 0.174* | |
C23 | 0.5236 (9) | 0.4096 (4) | 0.5899 (3) | 0.119 (2) | |
H23A | 0.461694 | 0.373742 | 0.585907 | 0.179* | |
H23B | 0.571500 | 0.427102 | 0.541999 | 0.179* | |
H23C | 0.474821 | 0.459559 | 0.605650 | 0.179* | |
C24 | 0.6820 (8) | 0.2730 (4) | 0.6269 (4) | 0.116 (2) | |
H24A | 0.712082 | 0.231179 | 0.670852 | 0.174* | |
H24B | 0.756538 | 0.280380 | 0.589885 | 0.174* | |
H24C | 0.613751 | 0.253751 | 0.607198 | 0.174* | |
C25 | 0.4674 (7) | 0.1584 (3) | 0.8899 (4) | 0.116 (2) | |
C29 | 0.4519 (4) | 0.6769 (2) | 0.6236 (2) | 0.0590 (8) | |
H29 | 0.453198 | 0.625371 | 0.610378 | 0.071* | |
C30 | 0.4229 (5) | 0.7543 (2) | 0.7128 (2) | 0.0660 (10) | |
H30 | 0.404673 | 0.757419 | 0.762635 | 0.079* | |
C31 | 0.4461 (5) | 0.8273 (3) | 0.6599 (3) | 0.0735 (12) | |
H31 | 0.444135 | 0.878111 | 0.674430 | 0.088* | |
C32 | 0.4773 (4) | 0.7477 (2) | 0.5680 (2) | 0.0589 (8) | |
H32 | 0.497842 | 0.742598 | 0.518731 | 0.071* | |
C33 | 0.4725 (4) | 0.8254 (2) | 0.5847 (2) | 0.0559 (8) | |
C34 | 0.4954 (4) | 0.9056 (2) | 0.5237 (2) | 0.0587 (8) | 0.669 (3) |
H34 | 0.518299 | 0.889879 | 0.475363 | 0.070* | 0.669 (3) |
C36 | 0.6090 (4) | 0.9449 (2) | 0.5407 (3) | 0.0643 (9) | 0.5 |
H36A | 0.690426 | 0.902169 | 0.544757 | 0.077* | 0.5 |
H36B | 0.586251 | 0.959916 | 0.588709 | 0.077* | 0.5 |
C37 | 0.6369 (4) | 1.0250 (2) | 0.4811 (2) | 0.0616 (9) | 0.169 (3) |
O6 | 0.6509 (17) | 0.9991 (9) | 0.4108 (4) | 0.061 (4) | 0.169 (3) |
H6A | 0.725788 | 0.970587 | 0.405440 | 0.091* | 0.169 (3) |
C34A | 0.4954 (4) | 0.9056 (2) | 0.5237 (2) | 0.0587 (8) | 0.331 (3) |
O6A | 0.5326 (8) | 0.8818 (5) | 0.4525 (3) | 0.0612 (19) | 0.331 (3) |
H6AA | 0.556336 | 0.922670 | 0.421105 | 0.092* | 0.331 (3) |
C36A | 0.6090 (4) | 0.9449 (2) | 0.5407 (3) | 0.0643 (9) | 0.5 |
H36C | 0.690426 | 0.902169 | 0.544757 | 0.077* | 0.5 |
H36D | 0.586251 | 0.959916 | 0.588709 | 0.077* | 0.5 |
C37A | 0.6369 (4) | 1.0250 (2) | 0.4811 (2) | 0.0616 (9) | 0.831 (3) |
H37A | 0.658257 | 1.009535 | 0.432665 | 0.074* | 0.831 (3) |
C38 | 0.7545 (4) | 1.0611 (2) | 0.4973 (3) | 0.0639 (9) | |
C39 | 0.7691 (5) | 1.0706 (3) | 0.5690 (3) | 0.0702 (10) | |
H39 | 0.704073 | 1.057652 | 0.608260 | 0.084* | |
C40 | 0.8814 (5) | 1.0995 (3) | 0.5800 (3) | 0.0825 (13) | |
H40 | 0.891593 | 1.103359 | 0.628146 | 0.099* | |
C41 | 0.9615 (5) | 1.1141 (3) | 0.4587 (4) | 0.0893 (15) | |
H41 | 1.026596 | 1.129588 | 0.420202 | 0.107* | |
C42 | 0.8540 (5) | 1.0840 (3) | 0.4423 (3) | 0.0785 (12) | |
H42 | 0.848586 | 1.079098 | 0.393866 | 0.094* | |
C43 | 0.5321 (5) | 0.5749 (3) | 0.9037 (3) | 0.0753 (11) | |
H43 | 0.449 (7) | 0.590 (4) | 0.925 (4) | 0.12 (2)* | |
C44 | 0.6459 (6) | 0.5596 (3) | 0.9428 (3) | 0.0866 (14) | |
H44 | 0.650 (6) | 0.540 (4) | 0.996 (3) | 0.101 (18)* | |
C45 | 0.6653 (4) | 0.5658 (3) | 0.7954 (3) | 0.0732 (11) | |
H45 | 0.666 (5) | 0.567 (3) | 0.747 (3) | 0.070 (13)* | |
C46 | 0.7798 (5) | 0.5519 (4) | 0.8306 (3) | 0.0853 (14) | |
H46 | 0.862776 | 0.545816 | 0.803159 | 0.102* | |
C47 | 0.7749 (6) | 0.5468 (3) | 0.9060 (3) | 0.0887 (15) | |
C48 | 0.9122 (7) | 0.5265 (4) | 0.9400 (4) | 0.113 (2) | 0.756 (3) |
H48 | 0.978986 | 0.541517 | 0.898050 | 0.136* | 0.756 (3) |
C49 | 0.9144 (5) | 0.5844 (3) | 0.9910 (3) | 0.0732 (11) | 0.5 |
H49A | 0.841263 | 0.577382 | 1.029863 | 0.088* | 0.5 |
H49B | 0.899764 | 0.643642 | 0.962548 | 0.088* | 0.5 |
C50 | 0.9499 (6) | 0.4346 (4) | 0.9716 (3) | 0.0971 (16) | 0.256 (3) |
O5 | 0.8318 (10) | 0.4167 (15) | 1.0216 (7) | 0.126 (8) | 0.256 (3) |
H5 | 0.833143 | 0.433524 | 1.059601 | 0.190* | 0.256 (3) |
C48A | 0.9122 (7) | 0.5265 (4) | 0.9400 (4) | 0.113 (2) | 0.244 (3) |
O5A | 1.0208 (13) | 0.5262 (8) | 0.8812 (6) | 0.168 (13) | 0.244 (3) |
H5A | 1.093135 | 0.516112 | 0.899608 | 0.253* | 0.244 (3) |
C49A | 0.9144 (5) | 0.5844 (3) | 0.9910 (3) | 0.0732 (11) | 0.5 |
H49C | 0.841263 | 0.577382 | 1.029863 | 0.088* | 0.5 |
H49D | 0.899764 | 0.643642 | 0.962548 | 0.088* | 0.5 |
C50A | 0.9499 (6) | 0.4346 (4) | 0.9716 (3) | 0.0971 (16) | 0.744 (3) |
H50A | 0.881643 | 0.420241 | 1.012912 | 0.117* | 0.744 (3) |
C51 | 0.9519 (5) | 0.3763 (3) | 0.9255 (3) | 0.0906 (15) | |
C53 | 0.8550 (5) | 0.3234 (4) | 0.9454 (3) | 0.227 (6) | |
H53 | 0.796397 | 0.325440 | 0.987965 | 0.273* | |
C55 | 0.8456 (7) | 0.2674 (4) | 0.9016 (5) | 0.339 (12) | |
H55 | 0.780736 | 0.231945 | 0.914839 | 0.407* | |
N4 | 0.9331 (8) | 0.2643 (4) | 0.8379 (5) | 0.226 (5) | |
C54 | 1.0300 (7) | 0.3172 (4) | 0.8181 (3) | 0.224 (6) | |
H54 | 1.088550 | 0.315171 | 0.775473 | 0.269* | |
C52 | 1.0394 (5) | 0.3732 (3) | 0.8619 (3) | 0.145 (3) | |
H52 | 1.104214 | 0.408667 | 0.848599 | 0.174* | |
C26 | 0.5244 (15) | 0.1520 (8) | 0.9660 (6) | 0.148 (6) | 0.5 |
H26A | 0.613822 | 0.165368 | 0.956704 | 0.223* | 0.5 |
H26B | 0.526787 | 0.094774 | 0.996580 | 0.223* | 0.5 |
H26C | 0.467788 | 0.192079 | 0.991420 | 0.223* | 0.5 |
C27 | 0.5482 (18) | 0.0906 (7) | 0.8540 (8) | 0.162 (7) | 0.5 |
H27A | 0.519589 | 0.097973 | 0.804992 | 0.242* | 0.5 |
H27B | 0.535465 | 0.034949 | 0.884022 | 0.242* | 0.5 |
H27C | 0.641736 | 0.095123 | 0.850003 | 0.242* | 0.5 |
C28 | 0.3207 (10) | 0.1460 (8) | 0.9091 (10) | 0.158 (6) | 0.5 |
H28A | 0.271327 | 0.191890 | 0.930287 | 0.237* | 0.5 |
H28B | 0.316869 | 0.092062 | 0.944594 | 0.237* | 0.5 |
H28C | 0.281990 | 0.146096 | 0.864359 | 0.237* | 0.5 |
C0AA | 0.6120 (10) | 0.1126 (9) | 0.8983 (10) | 0.166 (7) | 0.5 |
H0AA | 0.629478 | 0.066389 | 0.873152 | 0.249* | 0.5 |
H0AB | 0.625635 | 0.089984 | 0.950456 | 0.249* | 0.5 |
H0AC | 0.672178 | 0.152526 | 0.876510 | 0.249* | 0.5 |
C1AA | 0.3844 (19) | 0.1489 (12) | 0.9630 (8) | 0.184 (8) | 0.5 |
H1AA | 0.420578 | 0.096590 | 0.996782 | 0.276* | 0.5 |
H1AB | 0.293491 | 0.147248 | 0.955214 | 0.276* | 0.5 |
H1AC | 0.385791 | 0.196847 | 0.983909 | 0.276* | 0.5 |
C2AA | 0.408 (2) | 0.1208 (11) | 0.8353 (8) | 0.189 (7) | 0.5 |
H2AA | 0.312236 | 0.138210 | 0.837663 | 0.283* | 0.5 |
H2AB | 0.429646 | 0.059224 | 0.848897 | 0.283* | 0.5 |
H2AC | 0.445710 | 0.141590 | 0.785237 | 0.283* | 0.5 |
O7 | 1.1944 (5) | 1.1607 (5) | 0.5835 (5) | 0.165 (3) | |
H7 | 1.138692 | 1.155880 | 0.557064 | 0.247* | |
C56 | 1.1393 (11) | 1.2288 (6) | 0.6216 (7) | 0.194 (5) | |
H56A | 1.083786 | 1.206894 | 0.666228 | 0.233* | |
H56B | 1.083641 | 1.274877 | 0.588973 | 0.233* | |
C35 | 1.2515 (16) | 1.2617 (15) | 0.6423 (13) | 0.354 (15) | |
H35A | 1.330922 | 1.248793 | 0.610365 | 0.531* | |
H35B | 1.268326 | 1.234768 | 0.693484 | 0.531* | |
H35C | 1.228155 | 1.322749 | 0.636391 | 0.531* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0507 (3) | 0.0409 (3) | 0.0577 (3) | −0.00562 (17) | −0.00310 (19) | −0.00542 (18) |
O1 | 0.0825 (19) | 0.0565 (15) | 0.0739 (18) | −0.0109 (13) | −0.0022 (15) | −0.0201 (13) |
O2 | 0.0785 (18) | 0.0608 (15) | 0.0646 (16) | −0.0027 (13) | −0.0138 (14) | −0.0143 (13) |
O3 | 0.0696 (16) | 0.0501 (13) | 0.0604 (15) | −0.0065 (11) | 0.0027 (12) | −0.0104 (11) |
O4 | 0.0670 (17) | 0.0664 (16) | 0.0742 (18) | −0.0094 (13) | 0.0106 (14) | −0.0202 (14) |
N1 | 0.0545 (15) | 0.0411 (13) | 0.0547 (15) | −0.0090 (11) | −0.0057 (12) | −0.0060 (11) |
N2 | 0.068 (2) | 0.065 (2) | 0.132 (4) | −0.0149 (18) | −0.006 (2) | −0.026 (2) |
N3 | 0.0570 (17) | 0.0548 (16) | 0.0648 (19) | −0.0035 (13) | −0.0026 (14) | −0.0039 (14) |
C1 | 0.068 (2) | 0.0494 (18) | 0.061 (2) | −0.0117 (16) | −0.0015 (17) | −0.0064 (15) |
C2 | 0.065 (2) | 0.0503 (18) | 0.063 (2) | −0.0154 (16) | 0.0025 (17) | −0.0124 (15) |
C3 | 0.068 (2) | 0.062 (2) | 0.069 (2) | −0.0210 (18) | 0.0040 (19) | −0.0160 (18) |
C4 | 0.062 (2) | 0.074 (3) | 0.084 (3) | −0.0075 (19) | −0.008 (2) | −0.021 (2) |
C5 | 0.069 (3) | 0.064 (2) | 0.087 (3) | −0.0113 (19) | 0.001 (2) | −0.017 (2) |
C6 | 0.073 (3) | 0.059 (2) | 0.069 (2) | −0.0128 (18) | −0.0022 (19) | −0.0146 (18) |
C7 | 0.081 (3) | 0.075 (3) | 0.108 (4) | 0.010 (2) | −0.012 (3) | −0.030 (3) |
C8 | 0.172 (8) | 0.144 (7) | 0.118 (6) | 0.057 (6) | −0.011 (5) | −0.061 (5) |
C9 | 0.091 (5) | 0.161 (8) | 0.225 (10) | 0.010 (5) | 0.005 (6) | −0.097 (8) |
C10 | 0.282 (12) | 0.136 (7) | 0.131 (6) | 0.102 (7) | 0.016 (7) | −0.011 (5) |
C11 | 0.083 (3) | 0.084 (3) | 0.077 (3) | −0.027 (2) | −0.002 (2) | −0.022 (2) |
C12 | 0.118 (4) | 0.088 (3) | 0.104 (4) | −0.042 (3) | −0.002 (3) | −0.039 (3) |
C13 | 0.084 (3) | 0.105 (4) | 0.069 (3) | −0.020 (3) | 0.001 (2) | −0.018 (3) |
C14 | 0.086 (4) | 0.150 (6) | 0.105 (4) | −0.026 (4) | −0.018 (3) | −0.048 (4) |
C15 | 0.059 (2) | 0.0498 (18) | 0.070 (2) | −0.0082 (15) | 0.0040 (17) | −0.0104 (16) |
C16 | 0.0570 (19) | 0.0486 (17) | 0.061 (2) | −0.0068 (14) | −0.0022 (16) | −0.0090 (15) |
C17 | 0.070 (2) | 0.0508 (18) | 0.072 (2) | −0.0118 (17) | 0.0008 (19) | −0.0135 (17) |
C18 | 0.090 (3) | 0.050 (2) | 0.086 (3) | −0.006 (2) | 0.011 (2) | −0.014 (2) |
C19 | 0.097 (3) | 0.055 (2) | 0.085 (3) | −0.013 (2) | 0.015 (3) | −0.004 (2) |
C20 | 0.087 (3) | 0.065 (2) | 0.075 (3) | −0.018 (2) | 0.020 (2) | −0.006 (2) |
C21 | 0.094 (3) | 0.060 (2) | 0.073 (3) | −0.016 (2) | 0.013 (2) | −0.024 (2) |
C22 | 0.116 (5) | 0.116 (5) | 0.124 (5) | −0.047 (4) | 0.054 (4) | −0.053 (4) |
C23 | 0.188 (7) | 0.100 (4) | 0.067 (3) | −0.016 (5) | −0.009 (4) | −0.023 (3) |
C24 | 0.148 (6) | 0.081 (3) | 0.115 (5) | −0.015 (4) | 0.045 (4) | −0.044 (3) |
C25 | 0.147 (6) | 0.055 (3) | 0.125 (5) | −0.022 (3) | 0.018 (4) | 0.007 (3) |
C29 | 0.069 (2) | 0.0430 (16) | 0.063 (2) | −0.0133 (15) | −0.0011 (17) | −0.0089 (15) |
C30 | 0.088 (3) | 0.0514 (19) | 0.060 (2) | −0.0207 (18) | −0.0004 (19) | −0.0111 (16) |
C31 | 0.104 (3) | 0.0487 (19) | 0.071 (2) | −0.027 (2) | 0.003 (2) | −0.0130 (17) |
C32 | 0.065 (2) | 0.0478 (17) | 0.062 (2) | −0.0105 (15) | −0.0051 (17) | −0.0084 (15) |
C33 | 0.0586 (19) | 0.0447 (16) | 0.062 (2) | −0.0087 (14) | −0.0048 (16) | −0.0076 (14) |
C34 | 0.063 (2) | 0.0449 (17) | 0.064 (2) | −0.0108 (15) | −0.0017 (17) | −0.0065 (15) |
C36 | 0.059 (2) | 0.0481 (18) | 0.080 (3) | −0.0079 (15) | −0.0073 (18) | −0.0048 (17) |
C37 | 0.059 (2) | 0.0504 (18) | 0.071 (2) | −0.0100 (15) | 0.0004 (17) | −0.0077 (16) |
O6 | 0.065 (9) | 0.057 (8) | 0.055 (8) | −0.022 (7) | 0.003 (7) | 0.001 (6) |
C34A | 0.063 (2) | 0.0449 (17) | 0.064 (2) | −0.0108 (15) | −0.0017 (17) | −0.0065 (15) |
O6A | 0.060 (4) | 0.052 (4) | 0.066 (4) | −0.011 (3) | 0.004 (3) | −0.006 (3) |
C36A | 0.059 (2) | 0.0481 (18) | 0.080 (3) | −0.0079 (15) | −0.0073 (18) | −0.0048 (17) |
C37A | 0.059 (2) | 0.0504 (18) | 0.071 (2) | −0.0100 (15) | 0.0004 (17) | −0.0077 (16) |
C38 | 0.059 (2) | 0.0456 (17) | 0.079 (3) | −0.0051 (15) | −0.0017 (18) | −0.0057 (16) |
C39 | 0.077 (3) | 0.055 (2) | 0.078 (3) | −0.0101 (18) | −0.008 (2) | −0.0142 (19) |
C40 | 0.082 (3) | 0.060 (2) | 0.106 (4) | −0.005 (2) | −0.017 (3) | −0.021 (2) |
C41 | 0.066 (3) | 0.077 (3) | 0.123 (5) | −0.026 (2) | 0.009 (3) | −0.018 (3) |
C42 | 0.073 (3) | 0.065 (2) | 0.093 (3) | −0.020 (2) | 0.007 (2) | −0.013 (2) |
C43 | 0.077 (3) | 0.068 (3) | 0.074 (3) | −0.005 (2) | −0.002 (2) | −0.012 (2) |
C44 | 0.103 (4) | 0.076 (3) | 0.080 (3) | 0.000 (3) | −0.022 (3) | −0.020 (2) |
C45 | 0.054 (2) | 0.086 (3) | 0.074 (3) | −0.0046 (19) | −0.005 (2) | −0.015 (2) |
C46 | 0.059 (2) | 0.097 (4) | 0.099 (4) | 0.005 (2) | −0.014 (2) | −0.032 (3) |
C47 | 0.079 (3) | 0.083 (3) | 0.108 (4) | 0.014 (2) | −0.035 (3) | −0.037 (3) |
C48 | 0.113 (5) | 0.101 (4) | 0.133 (5) | 0.023 (4) | −0.056 (4) | −0.047 (4) |
C49 | 0.073 (3) | 0.068 (2) | 0.071 (3) | 0.007 (2) | −0.015 (2) | −0.013 (2) |
C50 | 0.0972 (18) | 0.0965 (18) | 0.0973 (18) | −0.0149 (10) | −0.0101 (10) | −0.0221 (10) |
O5 | 0.069 (8) | 0.21 (2) | 0.064 (8) | −0.053 (11) | −0.007 (6) | 0.047 (10) |
C48A | 0.113 (5) | 0.101 (4) | 0.133 (5) | 0.023 (4) | −0.056 (4) | −0.047 (4) |
O5A | 0.141 (16) | 0.34 (4) | 0.061 (9) | −0.17 (2) | 0.013 (10) | −0.027 (14) |
C49A | 0.073 (3) | 0.068 (2) | 0.071 (3) | 0.007 (2) | −0.015 (2) | −0.013 (2) |
C50A | 0.0972 (18) | 0.0965 (18) | 0.0973 (18) | −0.0149 (10) | −0.0101 (10) | −0.0221 (10) |
C51 | 0.076 (3) | 0.076 (3) | 0.120 (4) | −0.009 (2) | −0.031 (3) | −0.015 (3) |
C53 | 0.228 (7) | 0.218 (7) | 0.244 (7) | −0.048 (5) | −0.007 (5) | −0.067 (5) |
C55 | 0.341 (12) | 0.343 (12) | 0.342 (12) | −0.068 (5) | −0.025 (5) | −0.089 (6) |
N4 | 0.246 (6) | 0.217 (6) | 0.244 (6) | −0.054 (4) | −0.031 (5) | −0.087 (5) |
C54 | 0.220 (7) | 0.228 (7) | 0.218 (7) | −0.023 (5) | −0.020 (5) | −0.052 (5) |
C52 | 0.120 (6) | 0.186 (8) | 0.132 (6) | 0.034 (6) | −0.039 (5) | −0.076 (6) |
C26 | 0.179 (12) | 0.079 (7) | 0.149 (11) | −0.012 (8) | −0.019 (10) | 0.037 (7) |
C27 | 0.222 (15) | 0.053 (6) | 0.167 (13) | −0.002 (8) | 0.036 (12) | 0.012 (7) |
C28 | 0.194 (13) | 0.076 (7) | 0.181 (13) | −0.067 (8) | 0.037 (11) | 0.021 (9) |
C0AA | 0.192 (13) | 0.081 (8) | 0.175 (14) | 0.010 (9) | −0.007 (11) | 0.030 (9) |
C1AA | 0.223 (14) | 0.108 (9) | 0.164 (13) | −0.010 (11) | 0.059 (12) | 0.020 (10) |
C2AA | 0.244 (15) | 0.093 (9) | 0.198 (13) | −0.048 (10) | 0.021 (13) | 0.022 (10) |
O7 | 0.100 (4) | 0.213 (7) | 0.221 (7) | −0.013 (4) | −0.013 (4) | −0.134 (6) |
C56 | 0.235 (13) | 0.188 (11) | 0.193 (11) | −0.060 (10) | −0.032 (10) | −0.079 (9) |
C35 | 0.26 (2) | 0.48 (4) | 0.45 (3) | −0.17 (2) | 0.05 (2) | −0.31 (3) |
Geometric parameters (Å, º) top
Co1—O1 | 1.924 (3) | C34—C36 | 1.526 (6) |
Co1—O2 | 1.906 (3) | C34—C37i | 1.576 (5) |
Co1—O3 | 1.934 (3) | C36—H36A | 0.9700 |
Co1—O4 | 1.967 (3) | C36—H36B | 0.9700 |
Co1—N1 | 2.012 (3) | C36—C37 | 1.530 (5) |
Co1—N3 | 2.010 (4) | C37—O6 | 1.4504 (11) |
O1—C2 | 1.330 (5) | C37—C38 | 1.523 (6) |
O2—C1 | 1.328 (5) | O6—H6A | 0.8200 |
O3—C16 | 1.303 (4) | C34A—O6A | 1.4508 (11) |
O4—C15 | 1.298 (5) | C34A—C36A | 1.526 (6) |
N1—C29 | 1.343 (5) | O6A—H6AA | 0.8200 |
N1—C30 | 1.330 (5) | C36A—H36C | 0.9700 |
N2—C40 | 1.336 (7) | C36A—H36D | 0.9700 |
N2—C41 | 1.325 (8) | C36A—C37A | 1.530 (5) |
N3—C43 | 1.339 (6) | C37A—H37A | 0.9800 |
N3—C45 | 1.339 (6) | C37A—C38 | 1.523 (6) |
C1—C2 | 1.434 (6) | C38—C39 | 1.405 (6) |
C1—C6 | 1.384 (6) | C38—C42 | 1.377 (6) |
C2—C3 | 1.410 (6) | C39—H39 | 0.9300 |
C3—C4 | 1.387 (6) | C39—C40 | 1.372 (7) |
C3—C11 | 1.542 (6) | C40—H40 | 0.9300 |
C4—H4 | 0.9300 | C41—H41 | 0.9300 |
C4—C5 | 1.413 (7) | C41—C42 | 1.378 (7) |
C5—C6 | 1.386 (7) | C42—H42 | 0.9300 |
C5—C7 | 1.529 (6) | C43—H43 | 0.90 (7) |
C6—H6 | 0.9300 | C43—C44 | 1.389 (8) |
C7—C8 | 1.537 (9) | C44—H44 | 0.95 (6) |
C7—C9 | 1.522 (10) | C44—C47 | 1.403 (8) |
C7—C10 | 1.479 (5) | C45—H45 | 0.90 (5) |
C8—H8A | 0.9600 | C45—C46 | 1.358 (7) |
C8—H8B | 0.9600 | C46—H46 | 0.9300 |
C8—H8C | 0.9600 | C46—C47 | 1.372 (8) |
C9—H9A | 0.9600 | C47—C48 | 1.547 (8) |
C9—H9B | 0.9600 | C47—C48A | 1.547 (8) |
C9—H9C | 0.9600 | C48—H48 | 0.9800 |
C10—H10A | 0.9600 | C48—C49 | 1.500 (8) |
C10—H10B | 0.9600 | C48—C50 | 1.458 (9) |
C10—H10C | 0.9600 | C49—H49A | 0.9700 |
C11—C12 | 1.556 (8) | C49—H49B | 0.9700 |
C11—C13 | 1.531 (7) | C49—C50ii | 1.562 (8) |
C11—C14 | 1.530 (8) | C50—O5 | 1.4506 (11) |
C12—H12A | 0.9600 | C50—C51 | 1.427 (8) |
C12—H12B | 0.9600 | O5—H5 | 0.8200 |
C12—H12C | 0.9600 | C48A—O5A | 1.4506 (11) |
C13—H13A | 0.9600 | C48A—C49A | 1.500 (8) |
C13—H13B | 0.9600 | C48A—C50A | 1.458 (9) |
C13—H13C | 0.9600 | O5A—H5A | 0.8200 |
C14—H14A | 0.9600 | C49A—H49C | 0.9700 |
C14—H14B | 0.9600 | C49A—H49D | 0.9700 |
C14—H14C | 0.9600 | C49A—C50Aii | 1.562 (8) |
C15—C16 | 1.443 (5) | C50A—H50A | 0.9800 |
C15—C20 | 1.409 (6) | C50A—C51 | 1.427 (8) |
C16—C17 | 1.418 (5) | C51—C53 | 1.3900 |
C17—C18 | 1.375 (6) | C51—C52 | 1.3900 |
C17—C21 | 1.552 (6) | C53—H53 | 0.9300 |
C18—H18 | 0.9300 | C53—C55 | 1.3900 |
C18—C19 | 1.416 (7) | C55—H55 | 0.9300 |
C19—C20 | 1.361 (7) | C55—N4 | 1.3900 |
C19—C25 | 1.545 (6) | N4—C54 | 1.3900 |
C20—H20 | 0.9300 | C54—H54 | 0.9300 |
C21—C22 | 1.533 (8) | C54—C52 | 1.3900 |
C21—C23 | 1.535 (9) | C52—H52 | 0.9300 |
C21—C24 | 1.539 (7) | C26—H26A | 0.9600 |
C22—H22A | 0.9600 | C26—H26B | 0.9600 |
C22—H22B | 0.9600 | C26—H26C | 0.9600 |
C22—H22C | 0.9600 | C27—H27A | 0.9600 |
C23—H23A | 0.9600 | C27—H27B | 0.9600 |
C23—H23B | 0.9600 | C27—H27C | 0.9600 |
C23—H23C | 0.9600 | C28—H28A | 0.9600 |
C24—H24A | 0.9600 | C28—H28B | 0.9600 |
C24—H24B | 0.9600 | C28—H28C | 0.9600 |
C24—H24C | 0.9600 | C0AA—H0AA | 0.9600 |
C25—C26 | 1.561 (8) | C0AA—H0AB | 0.9600 |
C25—C27 | 1.491 (6) | C0AA—H0AC | 0.9600 |
C25—C28 | 1.529 (8) | C1AA—H1AA | 0.9600 |
C25—C0AA | 1.522 (8) | C1AA—H1AB | 0.9600 |
C25—C1AA | 1.490 (8) | C1AA—H1AC | 0.9600 |
C25—C2AA | 1.541 (8) | C2AA—H2AA | 0.9600 |
C29—H29 | 0.9300 | C2AA—H2AB | 0.9600 |
C29—C32 | 1.382 (5) | C2AA—H2AC | 0.9600 |
C30—H30 | 0.9300 | O7—H7 | 0.8200 |
C30—C31 | 1.378 (5) | O7—C56 | 1.4503 (11) |
C31—H31 | 0.9300 | C56—H56A | 0.9700 |
C31—C33 | 1.391 (6) | C56—H56B | 0.9700 |
C32—H32 | 0.9300 | C56—C35 | 1.480 (5) |
C32—C33 | 1.371 (5) | C35—H35A | 0.9600 |
C33—C34 | 1.532 (5) | C35—H35B | 0.9600 |
C33—C34A | 1.532 (5) | C35—H35C | 0.9600 |
C34—H34 | 0.9800 | | |
| | | |
O1—Co1—O3 | 87.26 (13) | C33—C34—C37i | 109.7 (3) |
O1—Co1—O4 | 92.27 (14) | C36—C34—C33 | 111.1 (3) |
O1—Co1—N1 | 87.97 (13) | C36—C34—H34 | 109.2 |
O1—Co1—N3 | 178.91 (13) | C36—C34—C37i | 108.4 (3) |
O2—Co1—O1 | 85.85 (13) | C37i—C34—H34 | 109.2 |
O2—Co1—O3 | 171.87 (13) | C34—C36—H36A | 108.9 |
O2—Co1—O4 | 91.89 (12) | C34—C36—H36B | 108.9 |
O2—Co1—N1 | 91.58 (13) | C34—C36—C37 | 113.3 (3) |
O2—Co1—N3 | 95.19 (13) | H36A—C36—H36B | 107.7 |
O3—Co1—O4 | 84.08 (11) | C37—C36—H36A | 108.9 |
O3—Co1—N1 | 92.48 (12) | C37—C36—H36B | 108.9 |
O3—Co1—N3 | 91.74 (13) | O6—C37—C36 | 104.5 (6) |
O4—Co1—N1 | 176.53 (11) | O6—C37—C38 | 116.0 (7) |
O4—Co1—N3 | 88.04 (14) | C38—C37—C36 | 112.5 (3) |
N3—Co1—N1 | 91.66 (13) | C37—O6—H6A | 109.5 |
C2—O1—Co1 | 110.2 (3) | O6A—C34A—C33 | 109.1 (4) |
C1—O2—Co1 | 109.7 (2) | O6A—C34A—C36A | 108.1 (4) |
C16—O3—Co1 | 112.0 (2) | C36A—C34A—C33 | 111.1 (3) |
C15—O4—Co1 | 110.4 (2) | C34A—O6A—H6AA | 109.5 |
C29—N1—Co1 | 122.2 (2) | C34A—C36A—H36C | 108.9 |
C30—N1—Co1 | 120.6 (3) | C34A—C36A—H36D | 108.9 |
C30—N1—C29 | 117.2 (3) | C34A—C36A—C37A | 113.3 (3) |
C41—N2—C40 | 116.2 (5) | H36C—C36A—H36D | 107.7 |
C43—N3—Co1 | 122.8 (3) | C37A—C36A—H36C | 108.9 |
C43—N3—C45 | 118.0 (4) | C37A—C36A—H36D | 108.9 |
C45—N3—Co1 | 118.8 (3) | C34Ai—C37A—H37A | 108.4 |
O2—C1—C2 | 117.4 (4) | C36A—C37A—H37A | 108.4 |
O2—C1—C6 | 123.0 (4) | C38—C37A—C34Ai | 110.7 (3) |
C6—C1—C2 | 119.6 (4) | C38—C37A—C36A | 112.5 (3) |
O1—C2—C1 | 115.1 (4) | C38—C37A—H37A | 108.4 |
O1—C2—C3 | 124.4 (4) | C39—C38—C37 | 122.1 (4) |
C3—C2—C1 | 120.5 (4) | C39—C38—C37A | 122.1 (4) |
C2—C3—C11 | 120.4 (4) | C42—C38—C37 | 121.3 (4) |
C4—C3—C2 | 116.7 (4) | C42—C38—C37A | 121.3 (4) |
C4—C3—C11 | 122.9 (4) | C42—C38—C39 | 116.6 (4) |
C3—C4—H4 | 117.8 | C38—C39—H39 | 120.7 |
C3—C4—C5 | 124.3 (4) | C40—C39—C38 | 118.5 (5) |
C5—C4—H4 | 117.8 | C40—C39—H39 | 120.7 |
C4—C5—C7 | 121.0 (4) | N2—C40—C39 | 124.7 (5) |
C6—C5—C4 | 117.3 (4) | N2—C40—H40 | 117.7 |
C6—C5—C7 | 121.6 (5) | C39—C40—H40 | 117.7 |
C1—C6—C5 | 121.6 (4) | N2—C41—H41 | 118.2 |
C1—C6—H6 | 119.2 | N2—C41—C42 | 123.6 (5) |
C5—C6—H6 | 119.2 | C42—C41—H41 | 118.2 |
C5—C7—C8 | 113.7 (5) | C38—C42—C41 | 120.4 (5) |
C9—C7—C5 | 110.3 (5) | C38—C42—H42 | 119.8 |
C9—C7—C8 | 100.5 (7) | C41—C42—H42 | 119.8 |
C10—C7—C5 | 111.3 (5) | N3—C43—H43 | 117 (4) |
C10—C7—C8 | 111.6 (7) | N3—C43—C44 | 121.2 (5) |
C10—C7—C9 | 108.9 (8) | C44—C43—H43 | 121 (4) |
C7—C8—H8A | 109.5 | C43—C44—H44 | 126 (4) |
C7—C8—H8B | 109.5 | C43—C44—C47 | 120.5 (5) |
C7—C8—H8C | 109.5 | C47—C44—H44 | 111 (4) |
H8A—C8—H8B | 109.5 | N3—C45—H45 | 114 (3) |
H8A—C8—H8C | 109.5 | N3—C45—C46 | 123.2 (5) |
H8B—C8—H8C | 109.5 | C46—C45—H45 | 123 (3) |
C7—C9—H9A | 109.5 | C45—C46—H46 | 119.5 |
C7—C9—H9B | 109.5 | C45—C46—C47 | 121.0 (5) |
C7—C9—H9C | 109.5 | C47—C46—H46 | 119.5 |
H9A—C9—H9B | 109.5 | C44—C47—C48 | 128.0 (6) |
H9A—C9—H9C | 109.5 | C44—C47—C48A | 128.0 (6) |
H9B—C9—H9C | 109.5 | C46—C47—C44 | 116.0 (5) |
C7—C10—H10A | 109.5 | C46—C47—C48 | 116.0 (5) |
C7—C10—H10B | 109.5 | C46—C47—C48A | 116.0 (5) |
C7—C10—H10C | 109.5 | C47—C48—H48 | 106.2 |
H10A—C10—H10B | 109.5 | C49—C48—C47 | 110.4 (5) |
H10A—C10—H10C | 109.5 | C49—C48—H48 | 106.2 |
H10B—C10—H10C | 109.5 | C50—C48—C47 | 111.2 (6) |
C3—C11—C12 | 109.7 (4) | C50—C48—H48 | 106.2 |
C13—C11—C3 | 110.0 (4) | C50—C48—C49 | 116.1 (5) |
C13—C11—C12 | 107.2 (5) | C48—C49—H49A | 109.1 |
C14—C11—C3 | 111.4 (5) | C48—C49—H49B | 109.1 |
C14—C11—C12 | 108.7 (5) | C48—C49—C50ii | 112.6 (4) |
C14—C11—C13 | 109.6 (5) | H49A—C49—H49B | 107.8 |
C11—C12—H12A | 109.5 | C50ii—C49—H49A | 109.1 |
C11—C12—H12B | 109.5 | C50ii—C49—H49B | 109.1 |
C11—C12—H12C | 109.5 | O5—C50—C48 | 101.2 (10) |
H12A—C12—H12B | 109.5 | C51—C50—C48 | 118.8 (5) |
H12A—C12—H12C | 109.5 | C51—C50—O5 | 99.5 (11) |
H12B—C12—H12C | 109.5 | C50—O5—H5 | 109.5 |
C11—C13—H13A | 109.5 | O5A—C48A—C47 | 110.1 (8) |
C11—C13—H13B | 109.5 | O5A—C48A—C49A | 115.6 (9) |
C11—C13—H13C | 109.5 | O5A—C48A—C50A | 92.4 (4) |
H13A—C13—H13B | 109.5 | C49A—C48A—C47 | 110.4 (5) |
H13A—C13—H13C | 109.5 | C50A—C48A—C47 | 111.2 (6) |
H13B—C13—H13C | 109.5 | C50A—C48A—C49A | 116.1 (5) |
C11—C14—H14A | 109.5 | C48A—O5A—H5A | 109.5 |
C11—C14—H14B | 109.5 | C48A—C49A—H49C | 109.1 |
C11—C14—H14C | 109.5 | C48A—C49A—H49D | 109.1 |
H14A—C14—H14B | 109.5 | H49C—C49A—H49D | 107.8 |
H14A—C14—H14C | 109.5 | C50Aii—C49A—H49C | 109.1 |
H14B—C14—H14C | 109.5 | C50Aii—C49A—H49D | 109.1 |
O4—C15—C16 | 117.4 (3) | C48A—C50A—H50A | 105.4 |
O4—C15—C20 | 123.2 (4) | C49Aii—C50A—H50A | 105.4 |
C20—C15—C16 | 119.4 (4) | C51—C50A—C48A | 118.8 (5) |
O3—C16—C15 | 116.0 (3) | C51—C50A—C49Aii | 110.2 (5) |
O3—C16—C17 | 123.8 (4) | C51—C50A—H50A | 105.4 |
C17—C16—C15 | 120.1 (3) | C53—C51—C50 | 116.1 (4) |
C16—C17—C21 | 120.5 (3) | C53—C51—C50A | 116.1 (4) |
C18—C17—C16 | 117.0 (4) | C53—C51—C52 | 120.0 |
C18—C17—C21 | 122.5 (4) | C52—C51—C50 | 123.8 (4) |
C17—C18—H18 | 118.1 | C52—C51—C50A | 123.8 (4) |
C17—C18—C19 | 123.8 (4) | C51—C53—H53 | 120.0 |
C19—C18—H18 | 118.1 | C55—C53—C51 | 120.0 |
C18—C19—C25 | 119.6 (4) | C55—C53—H53 | 120.0 |
C20—C19—C18 | 119.3 (4) | C53—C55—H55 | 120.0 |
C20—C19—C25 | 121.1 (5) | C53—C55—N4 | 120.0 |
C15—C20—H20 | 119.8 | N4—C55—H55 | 120.0 |
C19—C20—C15 | 120.4 (4) | C54—N4—C55 | 120.0 |
C19—C20—H20 | 119.8 | N4—C54—H54 | 120.0 |
C22—C21—C17 | 110.0 (4) | N4—C54—C52 | 120.0 |
C22—C21—C23 | 110.7 (5) | C52—C54—H54 | 120.0 |
C22—C21—C24 | 109.2 (5) | C51—C52—H52 | 120.0 |
C23—C21—C17 | 108.0 (4) | C54—C52—C51 | 120.0 |
C23—C21—C24 | 107.4 (5) | C54—C52—H52 | 120.0 |
C24—C21—C17 | 111.4 (4) | C25—C26—H26A | 109.5 |
C21—C22—H22A | 109.5 | C25—C26—H26B | 109.5 |
C21—C22—H22B | 109.5 | C25—C26—H26C | 109.5 |
C21—C22—H22C | 109.5 | H26A—C26—H26B | 109.5 |
H22A—C22—H22B | 109.5 | H26A—C26—H26C | 109.5 |
H22A—C22—H22C | 109.5 | H26B—C26—H26C | 109.5 |
H22B—C22—H22C | 109.5 | C25—C27—H27A | 109.5 |
C21—C23—H23A | 109.5 | C25—C27—H27B | 109.5 |
C21—C23—H23B | 109.5 | C25—C27—H27C | 109.5 |
C21—C23—H23C | 109.5 | H27A—C27—H27B | 109.5 |
H23A—C23—H23B | 109.5 | H27A—C27—H27C | 109.5 |
H23A—C23—H23C | 109.5 | H27B—C27—H27C | 109.5 |
H23B—C23—H23C | 109.5 | C25—C28—H28A | 109.5 |
C21—C24—H24A | 109.5 | C25—C28—H28B | 109.5 |
C21—C24—H24B | 109.5 | C25—C28—H28C | 109.5 |
C21—C24—H24C | 109.5 | H28A—C28—H28B | 109.5 |
H24A—C24—H24B | 109.5 | H28A—C28—H28C | 109.5 |
H24A—C24—H24C | 109.5 | H28B—C28—H28C | 109.5 |
H24B—C24—H24C | 109.5 | C25—C0AA—H0AA | 109.5 |
C19—C25—C26 | 107.2 (6) | C25—C0AA—H0AB | 109.5 |
C27—C25—C19 | 114.7 (7) | C25—C0AA—H0AC | 109.5 |
C27—C25—C26 | 109.2 (7) | H0AA—C0AA—H0AB | 109.5 |
C27—C25—C28 | 111.9 (7) | H0AA—C0AA—H0AC | 109.5 |
C28—C25—C19 | 107.4 (6) | H0AB—C0AA—H0AC | 109.5 |
C28—C25—C26 | 106.0 (6) | C25—C1AA—H1AA | 109.5 |
C0AA—C25—C19 | 109.2 (7) | C25—C1AA—H1AB | 109.5 |
C0AA—C25—C2AA | 107.4 (7) | C25—C1AA—H1AC | 109.5 |
C1AA—C25—C19 | 116.0 (9) | H1AA—C1AA—H1AB | 109.5 |
C1AA—C25—C0AA | 112.4 (7) | H1AA—C1AA—H1AC | 109.5 |
C1AA—C25—C2AA | 110.7 (7) | H1AB—C1AA—H1AC | 109.5 |
C2AA—C25—C19 | 100.0 (8) | C25—C2AA—H2AA | 109.5 |
N1—C29—H29 | 118.7 | C25—C2AA—H2AB | 109.5 |
N1—C29—C32 | 122.6 (3) | C25—C2AA—H2AC | 109.5 |
C32—C29—H29 | 118.7 | H2AA—C2AA—H2AB | 109.5 |
N1—C30—H30 | 118.5 | H2AA—C2AA—H2AC | 109.5 |
N1—C30—C31 | 123.0 (4) | H2AB—C2AA—H2AC | 109.5 |
C31—C30—H30 | 118.5 | C56—O7—H7 | 109.5 |
C30—C31—H31 | 119.9 | O7—C56—H56A | 109.9 |
C30—C31—C33 | 120.2 (4) | O7—C56—H56B | 109.9 |
C33—C31—H31 | 119.9 | O7—C56—C35 | 108.9 (10) |
C29—C32—H32 | 119.7 | H56A—C56—H56B | 108.3 |
C33—C32—C29 | 120.6 (4) | C35—C56—H56A | 109.9 |
C33—C32—H32 | 119.7 | C35—C56—H56B | 109.9 |
C31—C33—C34 | 122.0 (3) | C56—C35—H35A | 109.5 |
C31—C33—C34A | 122.0 (3) | C56—C35—H35B | 109.5 |
C32—C33—C31 | 116.4 (3) | C56—C35—H35C | 109.5 |
C32—C33—C34 | 121.5 (3) | H35A—C35—H35B | 109.5 |
C32—C33—C34A | 121.5 (3) | H35A—C35—H35C | 109.5 |
C33—C34—H34 | 109.2 | H35B—C35—H35C | 109.5 |
Symmetry codes: (i) −x+1, −y+2, −z+1; (ii) −x+2, −y+1, −z+2. |
Selected geometric parameters (Å, °) for the Co coordination sphere in
1.7EtOH.5H2O and 2.EtOH.nH2O top1.7EtOH.5H2O | | | 2.EtOH.nH2O | | |
| | | 100 K | 275 K | 315 K |
| | | (n = 5) | (n = 5) | (n = 3) |
Co1—O1 | 1.907 (3) | Co1—O1 | 1.863 (3) | 1.860 (2) | 1.924 (3) |
Co1—O2 | 1.891 (3) | Co1—O2 | 1.880 (3) | 1.865 (2) | 1.906 (3) |
Co1—O3 | 1.854 (3) | Co1—O3 | 1.905 (2) | 1.893 (2) | 1.934 (3) |
Co1—O4 | 1.884 (3) | Co1—O4 | 1.917 (2) | 1.912 (2) | 1.967 (3) |
Co1—N1 | 1.953 (4) | Co1—N1 | 1.941 (3) | 1.953 (2) | 2.012 (3) |
Co1—N2i | 1.964 (3) | Co1—N3 | 1.955 (3) | 1.960 (3) | 2.010 (4) |
| | | | | |
O3—Co1—O2 | 87.67 (11) | O1—Co1—O2 | 88.39 (11) | 87.35 (10) | 87.26 (13) |
O3—Co1—O1 | 87.02 (12) | O1—Co1—O3 | 88.19 (11) | 88.02 (10) | 92.27 (14) |
O3—Co1—O4 | 87.97 (12) | O1—Co1—O4 | 91.63 (12) | 91.56 (11) | 87.97 (13) |
O3—Co1—N1 | 87.73 (13) | O1—Co1—N1 | 88.40 (11) | 88.70 (10) | 178.91 (13) |
O3—Co1—N2i | 178.92 (15) | O1—Co1—N3 | 178.52 (11) | 178.52 (11) | 85.85 (13) |
O2—Co1—O1 | 85.29 (11) | O2—Co1—O3 | 175.44 (11) | 174.26 (10) | 171.87 (13) |
O2—Co1—N1 | 174.65 (12) | O2—Co1—O4 | 90.99 (11) | 91.60 (10) | 91.89 (13) |
O2—Co1—N2i | 92.60 (13) | O2—Co1—N1 | 90.96 (11) | 90.98 (11) | 91.58 (13) |
O1—Co1—N1 | 91.75 (14) | O2—Co1—N3 | 92.99 (11) | 94.11 (11) | 95.19 (13) |
O1—Co1—N2i | 94.05 (14) | O3—Co1—O4 | 86.09 (10) | 85.13 (10) | 84.08 (11) |
O4—Co1—O2 | 89.55 (12) | O3—Co1—N1 | 91.96 (11) | 92.27 (10) | 92.48 (12) |
O4—Co1—O1 | 172.94 (11) | O3—Co1—N3 | 90.46 (11) | 90.54 (11) | 91.74 (13) |
O4—Co1—N1 | 93.01 (15) | O4—Co1—N1 | 178.05 (11) | 177.37 (10) | 176.53 (11) |
O4—Co1—N2i | 90.99 (14) | O4—Co1—N3 | 88.89 (12) | 88.62 (11) | 88.04 (14) |
N1—Co1—N2i | 92.05 (14) | N1—Co1—N3 | 91.04 (12) | 91.06 (11) | 91.66 (13) |
Symmetry code: (i) x, -y+1/2, z-1/2. |
Selected bond lengths (Å) for the dioxolene ligands in
1.2EtOH.15H2O and 2.EtOH.nH2O top1.7EtOH.5H2O | | | 2.EtOH.nH2O | | |
| | | 100 K | 275 K | 315 K |
| | | (n = 5) | (n = 5) | (n = 3) |
O1—C1 | 1.313 (4) | O1—C2 | 1.343 (4) | 1.333 (4) | 1.330 (5) |
O1—C2 | 1.316 (4) | O2—C1 | 1.341 (4) | 1.326 (4) | 1.328 (5) |
O3—C15 | 1.338 (5) | O3—C16 | 1.307 (4) | 1.294 (3) | 1.303 (4) |
O4—C16 | 1.356 (5) | O4—C15 | 1.305 (4) | 1.289 (4) | 1.298 (5) |
C1—C2 | 1.441 (5) | C1—C2 | 1.423 (5) | 1.399 (5) | 1.434 (6) |
C3—C2 | 1.438 (5) | C1—C6 | 1.397 (5) | 1.379 (5) | 1.384 (6) |
C4—C3 | 1.369 (5) | C2—C3 | 1.408 (5) | 1.387 (5) | 1.410 (6) |
C4—C5 | 1.432 (5) | C3—C4 | 1.405 (5) | 1.387 (5) | 1.387 (6) |
C6—C5 | 1.371 (5) | C4—C5 | 1.419 (5) | 1.386 (5) | 1.413 (7) |
C1—C6 | 1.394 (5) | C5—C6 | 1.391 (5) | 1.382 (5) | 1.386 (7) |
C15—C16 | 1.408 (5) | C15—C16 | 1.447 (5) | 1.434 (4) | 1.443 (5) |
C16—C17 | 1.386 (6) | C15—C20 | 1.406 (4) | 1.391 (4) | 1.409 (6) |
C17—C18 | 1.406 (6) | C16—C17 | 1.427 (4) | 1.404 (4) | 1.418 (5) |
C19—C18 | 1.398 (6) | C17—C18 | 1.388 (4) | 1.364 (5) | 1.375 (6) |
C20—C19 | 1.405 (6) | C18—C19 | 1.418 (5) | 1.403 (5) | 1.416 (7) |
C15—C20 | 1.415 (5) | C19—C20 | 1.380 (5) | 1.361 (5) | 1.361 (7) |
The distances within dioxolene are indicative of the oxidation state of the
ligand, e.g. the average C—O distance for semiquinone is
1.285 (13) Å, while for catecholate, this value should be close to
1.355 (15) Å (Mulyana et al., 2010). |